Kraft Green Liquor Pulping of Douglas-Fir for Corrugating Medium

AN ABSTRACT OF THE THESIS OF

YI-PYGN FANG for the degree of MASTER OF SCIENCE in FOREST PRODUCTS presented on Xi?VI /5 /PIO Title: KRAFT GREEN LIQUOR PULPING OF DOUGLAS-FIR

FOR CORRUGATING MEDIUM

Abstract approved: Redacted for Privacy (1/4Talter Tj. Bublit6

Douglas-fir wood chips from Oregon were pulped with kraft green liquor to produce semi-chemical pulps with properties suitable for the manufacture of corrugating medium.The effects of five cooking variables were studied, chemical charge, chip size, bark content of chips, pulping temperature, and liquor sulfidity.The combinations of levels of these five independent variables were chosen according to an incomplete block design, which allowed a maximum amount of statistical information to be obtained from only 30 individual cooks. Pulping properties studied were pulp yield, total solids of the waste liquor, pH of the waste liquor, the hypo number test of the pulp, and such pulp strength properties as Concora crush strength, tensile, burst, tear, and stiffness.Chemical charge is the most important single variable affecting pulp yield, tensile strength, and Concora strength, whereas the salfidity does not affect the pulp yield but does affect the tensile and Concora strengths.Cooking temperature, bark content, and chip size have less significant effects on pulp yields and pulp strength properties.Green liquor pulps have distinctly darker colors than neutral sulfite pulps from the same wood species, and the former pulp forms denser sheets than the latter. Generally speaking, green liquor semi-chemical Douglas-fir pulps are equivalent to or slightly lower in quality than other commercial semi-chemical pulps in Concora strength, but equal or slightly superior to them in tensile and bursting strengths.The deficiency in Concora strength can be overcome with increased refining, and the slightly higher pulp yield and elimination of the causticizing step make the green liquor semi-chemical process more attractive for corrugating medium. .444 Kraft Green Liquor Pulping of Douglas-fir for Corrugating Medium

by Yi-Pygn Fang

A THESIS submitted to Oregon State University

in partial fulfillment of the requirements for the degree of Master of Science June 1977 APPROVED:

Redacted for Privacy

< ear Associate Professorfrf Forest Products in charge of major

Redacted for Privacy

Headobiepartment of Forest Productsi

Redacted for Privacy

Dean of Graduate Schlool

Date thesis is presented je"/4096 Typed by Opal Grossnicklaus for Yi-Pygn Fang ACKNOWLEDGEMENT

The writer wishes to express his sincere and deep appreciation to his major professor, Dr. Walter J. Bublitz, for his encouragement and competent guidance and untiring help throughout the study.With- out his help and support, this thesis would never have been possible. Special thanks are extended to Dr. Kenneth Rowe of the Oregon State University Statistics Department for his assistancewith statistical analysis and to Dr. Murray Laver for his kind assistanceand

encouragement. The writer extends his appreciation to Jerry L. Hullfor his help and suggestions regarding experimental procedure. The writer is deeply grateful to his parents for theirunderstand- ing and encouragement of his study in the United States. The deepest gratitude is expressed to Irene for her help and encouragement. TABLE OF CONTENTS

INTRODUCTION LITERATURE REVIEW Corrugating Me dium Kraft Process 5 Neutral Sulfite Semi -Chemical (NSSC) Process 6 Cross Recovery 9 Green Liquor Semi-Chemical (GLSC) Process 11 Experimental Design 18

EXPERIMENTAL PROCEDURE 22

Material Flow Sheet 22 Sample Selection 23 Sample Preparation 23 Chips 23 Chemical Treatment 25 Preparation of Cooking Liquor 25 Cooking Conditions 26 Hypo Number Test 28 Chip Disintegration 29 Pulp Refining 30 Handsheet Formation 31 Handsheet Testing 31

RESULTS AND DISCUSSION 34

Sample Preparation 34 Pulping Results 34 Total Solids in Waste Liquor 35 pH Value of Waste Liquor 35 Pulp Yield 38 Hypo Number Test 38 Chip Disintegration and Pulp Refining 43 Clearance Determination 43 Power Consumption and Initial Freeness 44 PFI Refiner 45 Pulp Quality 46 Introduction 46 Concora Strength 47 Tensile Strength 50 Bursting Strength 53 Tearing Strength 57 Stiffness (MOE) 57 Freeness, Bulk, and PFI Revolutions 60 Stiffness and Coricora Strength 65 Comparison of Different Semi-Chemical Pulps 66 GLSC and NSSC Softwood 66 GLSC and NSSC Hardwood 66

SUMMARY 69

CONCLUSIONS 73

BIBLIOGRAPHY 76

APPENDIX 79 LIST OF FIGURES

Figure Page

Simplified diagram of the kraft recovery process. 7 Simplified block diagram of the cross-recovery process. 10 Diagram showing cyclic nature of the kraft recovery process and GLSC process. 13 Flow sheet of materials (experimental procedure) 22 LIST OF TABLES Table Page

Cooking conditions. 19

Experimental plan. 21

. Summary of physical tests. 33

Size and classification of Douglas-fir chips. 34

Multiple regression of cooking variables to pulping results. 36

Predicted maximum value of pulping results. 37 Hypo number test. 40 Hypo number vs. beating revolution (PFI). 42 Hypo number vs. beating revolution (PFI). 42 9-1. Hypo number vs. beating revolution (PFI). 42 Disintegration data. (Bauer Refiner). 43 Power consumption. 44 Refining data. (PFI mill) 45 Multiple regression of cooking variables to Concora strength. 48 Predicted maximum value of pulp properties. (Concora strength, Bursting strength, and Tensile strength) 51 Multiple regression of cooking variables to Breaking length. 54 Multiple regression of cooking variables to Burst factor. 55

17. Multiple regression of cooking variables to Tear factor. 58 Table Page 17-1.Predicted maximum value of pulp properties. (Tear factor, Stiffnes (MOE), Bulk, Freeness, and PFI Revolution) 59 Multiple regression of cooking variables to stiffness (MOE). 61 Multiple regression of cooking variables to Freeness, ml CSF. 62 Multiple regression of cooking variables to bulk. 63 Multiple regression of cooking variables to PFI revs. 64 Comparison of QLSC and NSSC softwood corrugating medium- handsheet data. 67 Comparison of GLSC and NSSC hardwood corrugating medium - handsheet data. 68 LIST OF APPENDIX TABLES Appendix Table Page

Simple linear regression of pulp qualities. 79 Multiple regression equations relating cooking variables to pulping results. 80 Multiple regression equations relating cooking variables to pulp properties (200 ml CSF level). 81 Multiple regression equations relating cooking variables to pulp properties (1,000 PFI revolutions level). 83 Multiple regression equations relating cooking variables to pulp properties (1. 8 cc/gm Bulk level). 85 Multiple regression equations relating cooking variables to pulp properties (0 PFI revolutions level). 87

7, Original data. 89 KRAFT GREEN LIQUOR PULPING OF DOUGLAS-FIR FOR CORRUGATING MEDIUM

INTRODUCTION

Corrugating medium, the inner, fluted portion of a corrugated box, is a major commodity in the pulp and paper industry.Corru- gated boxes are an important item in all industries, and have shown steady growth over the past decade with a projected continuation of this growth rate. Traditionally, most corrugating medium has been manufactured by the neutral sulfite semi-chemical process (NSSC process), but witli the advent of more stringent pollution laws, dumping of the untreated NSSC waste liquor into rivers or the ocean is prohibited. Chemical recovery processes have been developed for NSSC liquors, but they are tediuos, complex, and involve significant capital investment.Very few such processes have been installed commercially. In recent years, a hybrid recovery process called "cross- recovery" has been developed for recovery of NSSC waste liquors in a kraft mill recovery system.The NSSC mill "sells" its waste liquor to the kraft mill, and the NSSC chemicals become the make-up chemical for the kraft recovery system, thus avoiding dumping of the untreated NSSC waste liquor and simultaneously furnishing make- up chemical for the kraft mill.The two mills must be located on the same site, or very close to each other, and in addition to various operating problems in the kraft recovery mill, there is a further restriction of the output of the NSSC mill based on the kraft mill output.While it has proved feasible in many cases, it is thus not a universal answer to the problems of corrugating mediummanufac- ture. Kraft green liquor, which is the intermediate stage of conversion of kraft white liquor from kraft black liquor, has been the subject of investigation in recent years for the manufacture of corrugating medium.It is a milder pulping chemical than kraft white liquor, and theoretically should be obtainable in any quantity from a kraft recovery system without upsetting the chemical balance.The field is relatively new and untapped, and considerably more information should be obtained to put this concept of pulping into proper perspec- tive. Hardwood species have been traditionally used for corrugating medium, but in recent years various softwoods such as Georgia pine and Douglas-fir have been utilized as mills have discovered proper methods of pulping these species.Douglas-fir, because of its preva- lence and good structural qualities, is the major lumber species in the Pacific Northwest region, and thus Douglas-fir chips produced as a residual material from the manufacture oflumber are the com- monest and one of the cheapest fiber sources in this region.For these reasons, Douglas-fir was chosen for this project as the source of wood for the kraft green liquor semi-chemical pulping process for the manufacture of corrugating medium. The basic objectives of this project:

. To study the effect of chemical charge, chip size, bark content, cooking temperature, and liquor sulfidity on green liquor pulping of Douglas-fir for corrugating medium.

2,To investigate the cooking conditions for optimizing pulp properties desirable for corrugating medium. LITERATURE REVIEW

Kraft green liquor has been studied recently as an alternative chemical to NSSC liquor for production of corrugating medium with good success (Worster, 1973).It is a milder pulping material than kraft white liquor and seems to impart the desired qualities to the semi-chemical pulp for the production of corrugating medium. Only a few articles have been published regarding green liquor pulping for semi-chemical pulps, including articles by Vardheim of Defibrator Aktiebolag (1967), Yerger of Owens-Illinois (1972), Worster (1973), Battan, Ahlquist and Snyder (1975), Charbonnier, Rushton and Schwalbe (1974), and Dawson (1974).No mention has been made in these articles of green liquor pulping on Douglas-fir for corrugating medium.

Corrugating Medium

Corrugating medium, the inner, fluted portion of a corrugated box, is a major commodity in the pulp and paper industry.Corru- gated boxes are an important item in all industries, being used for the shipping of materials as diverse as heavy machinery to food, and this segment of the paper industry has shown steady growth over the past decade with a projected continuation of this growth rate.Rebeck (1973) reported that the corrugated box industry has an average rate 5 of growth of 5. 7 percent per year for the ten year period from1963 to 1972.Pollitzer (1972) reported that in the U. S. about 4.3 million tons of corrugating medium are produced annually.At a price of $200 per ton, this represents an income of $860 million nationally. Corrugating medium is normally made by a high-yieldpulping process from a variety of woods, andhardwoods have been traditionally favored for this product.In recent years various softwoods such as Douglas-fir and southern pine have beenutilized as mills have discovered proper methods of pulping thesespecies. Properties of corrugating medium and corrugatingboards made from NSSC, GLSC, and Kraft SC pulps were coveredby Chides ter (1969), Becker and Galdwell (1974), Charbonnier (1974),Dawson (1974), and Battan et al.(1975).

Kraft Process

In the kraft (sulfate) process a mixture of sodiumsulfide (Na2S) and sodium hydroxide (NaOH) is used to pulp the wood toproduce a pulp of high quality.Sodium sulfate (Na2S04) is used as a make-up chemical to replace any chemical losses during pulpingand liquor recovery. The major inorganic reactions of liquor components were discussed by Wenzl (1967), Whitney (1968), and Clayton(1969). The reactions of the cooking chemicals with lignin were reported by Clayton (1968), and Wenzl (1967). Spent liquors from the kraft process (black liquor) are recov- ered through the recovery system which includes the multiple effect evaporator, recovery furnace, and causticizing requirement.This operation is discussed by Wenzl (1967), Whitney (1968), Casey (1961), and Tomlinson and Richter (1969). The chemical losses (sodium salt) in the kraft process might normally be between 5 and 15% of the total amount circulating.Sod- ium sulfate (Na2SO4) as the make-up chemical is added to theheavy black liquor prior to incineration being subsequently reduced inthe recovery furnace by the carbon monoxide. A simplified diagram which illustrates the cyclic natureof the kraft recovery process is shown in Fig1.

Neutral Sulfite Semi-Chemical (NSSC) Process

Semi-chemical pulping is a two-stage pulping process; in the first stage a mild chemical treatment is used forpartial removal of lignin and hemicellulose to weaken the intercellular bondingof chips, followed by mechanical treatment to separate the individualfibers. Because of the mild nature of the pulping chemicals and the short cooking time, the pulp yield is relatively high, usually about60 to 80% (Chidester, 1969). Traditionally, most corrugating medium has been manufactured chips water

white liquor mud washer digester S + NaOH ( CaCO3 ) (Na2 NI weak black liquor clarifier mud (R-ONa, R-SH, R-SNa) thickener

CaCO3 causticizer lime kiln [Ca(OH)2 + Na2C 2 Na0+ CaCO

CaO-"t

green liquor (Na2CO3 + Na2S)

evaporator

strong black liquor green liquor clarifier dregs dissolving tank washer

smelt weak liquor makeup chemical recovery furnace ) (Na2 SO4 4 (Na2 SO4 + CO Na2S +CO2) A (R-ONa - Na2 CO3 + heat)

Fig. 1 Simplified diagram of the kraft recovery process. by the NSSC process which was developed in the 1930 s (Worster, 1973; Chidester, 1969).In this process, the wood chips are pulped with a solution of sodium sulfite (Na2SO3) containingsmall amounts of an alkaline agent such as sodium hydroxide (NaOH), sodiumcarbon- ate (Na2CO3), or sodium bicarbonate (NaHCO3) forrelatively short periods of time, varying from 15 to 60 minutes.Some lignin and hemicellulose are removed through sulfonation and hydrolysis,and the rigid matrix in which the wood fibers are boundtogether is softened. After washing, the cooked chips, which are still quitehard due to the high lignin content, are sent to a diskmill for disintegrating. Further refining is usually needed to develop the necessarypulp properties for the end product. Spent liquors from NSSC mills do not contain manycompounds specifically toxic to aquatic life, but because of the deep colorand biodegradable material that can consume dissolved oxygen in water, they are objectionable if dumped untreated into streamsof limited

flow. NSSC spent liquor can be collected, evaporated, burned,and converted back into fresh NSSC liquor in a mannersimilar to the kraft recovery process that has proven so successful. The pulping process and properties of NSSC pulps arecovered by Casey (1966), Rydholm (1967), Chidester(1969), and 9

McGovern (1962).

Cross Recovery

The chemistry of the NSSC recovery process isconsiderably more complex than that of the kraft process,and the heat value per pound of solids of NSSC spent liquor is lower than that of the kraft spent liquor (6 to 12 million Btu for NSSC vs.21 million for kraft per ton of pulp produced) (Chidester,1969; Wenzl, 1967).Thus capital investments are higher and the process is much more difficult to control than the kraft recovery process.Because of the low initial cost of the cooking chemicals, sulfur and caustic, there hasbeen little economic incentive for the high capital expenditure for recovery plants. In recent years, an economical and effective methodadopted by a number of mills in the industry is that of cross-recovery (Worster, 1973; Chidester, 1969) in which both NSSCand kraft operations are conducted at the same site.The kraft mill is built conventionally, except that the recovery system isdesigned larger than necessary for a lone kraft mill, of the same pulpcapacity. The spent NSSC liquors are introduced to the kraft recovery system, where they are evaporated, burned, causticized,and converted to kraft white liquor.The sulfur (S) and soda (NaOH) obtained from NSSC spent liquor can be considered as a source of make-up 10 pulping chemicals for the kraft process, and it replacesthe tradi-

tional source of this material, namely salt cake (Na2 SO4). The kraft mill credits the NSSC mill for the value of thesechemicals supplied, which partially offsets the cost of fresh sulfur andalkali for the NSSC mill.The NSSC mill buys fresh raw material for pulpingand pre- pares fresh cooking liquorfor each batch.. A simplified diagram which illustrates the cross-recovery

process is shown in Fig.2.

KRAFT MILL NSSC MILL

White liquor Digester Fresh chemicals

Causticizing Weak 'black Digester department liquor

Weak spent liquor,as makeup chemicals Recovery furnace Evaporator for kraft process

Fig.2.Simplified block diagram of the cross-recovery process.

In the cross-recovery process, thechemical balance of the system may be perfect, or there maybe an excess of chemicals coming from the NSSC process to supplymake-up chemicals for the In the cross-recovery process, the chemical balance of the system may be perfect, or there may be an excess of chemicals coming from the NSSC process to supply make-up chemicals for the kraft process.To utilize all of the chemical from the NSSC spent liquor, the kraft mill should have about three times the pulp capacity of the NSSC mill (Chidester, 1969).Otherwise, the mill (kraft) must dis- pose of its excess liquor, usually the green liquor.This is done by the Western Kraft Co. mill in Albany, Oregon, which sells its excess green liquor to other kraft mills.Production of NSSC pulp in excess Of this limit leads to operating problems in the kraft recovery plant, such as high liquor viscosity, imbalance of the sodium-sulfur ratio, lower heat value per pound of spent liquor solids (due to the lower organic content of the NSSC spent liquor), which makes it more difficult to maintain combustion in the recovery furnace.

Green Liquor Semi-Chemical (GLSC) Process

During recent years kraft green liquor has been considered as an alternative chemical to NSSC liquor in the semi-chemical pulping process for producing corrugating medium.The GLSC process has several advantages over the NSSC process in a cross-recovery situa- tion.

1.There should be no restrictions to the ratio of semi-chemical to kraft pulp production.Based on actual commercial practice 1 2

at the Georgia-Pacific mill in Toledo, Oregon, the organic- inorganic ratio and the sodium-sulfur ratio of the semi-chemical spent liquors are very similar to those of the kraft spent liquors, and thus the operation of the recovery system is not affected by burning the semi-chemical spent liquors in any proportion.

. The green liquor process could be installed in an existing kraft mill with little or no modification of existing equipment, assum- ing the recovery boiler and evaporator are large enough.

3.Capital investment for a green liquor pulping facility would be somewhat less than that for a comparable capacity kraft mill, and substantially below that for a NSSC mill with independent recovery.

. The pulp mill making the medium does not need to purchase fresh pulping chemicals. Fig. 3 illustrates the cyclical nature of the kraft and GLSC processes. Vardheim (1967) has published the most definitive article, justifying the idea on the basis of reduced water pollution compared to a NSSC mill.He reported that mill production material was comparable in quality to standard NSSC medium, with the exception of darker color and slight odor to the green liquor medium. Yerger (1972) reported that a variety of treated green liquors were used to prepare corrugating medium, and that the latter were comparable in quality white liquor chips causticizing department

digester green liquor digeste cooked chips pulp KRAFT MILL recovery GLSC MILL furnace

weak black evaporator spe t liquor liquor

Fig.3.Diagram showing cyclic nature of the kraft recovery process and GLSC process. 14 with commercial NSSC medium. A German patent of Cederquistand Defibrator (1973) reported that "GLSC spent liquor is thickened and subjected to combustion to give a Na sulfide and Na carbonate smelt, which is dissolved in water for the preparation of new cooking liquor. " Considerable work has been done in eastern Europe (Szwarcsztajn, 1968; Lyubavskaya and Sazonova, 1971), but the information published

is sketchy.Worster (1973) reveiwed recent developments in semi- chemical pulping and stated "The green liquor pulping processhas a very low capital costcompared to sodium base NSSC pulping and is particularly attractive for an integrated NSSCkraft mill. It Dawson (1974) reported that, in the laboratoryevaluation of green liquor semichemica.1 hardwood(predominantly oak and gum) pulp, tensile strength and Concora strengthof GLSC pulps were similar to those of Olinkraft's NSSC pulps at 75% yield.A possible exception may be that the tensile strength of the GLSCtends to drop off below 200 CSF, whereas the NSSC pulp does not.Less chemicals were required with green liquor pulping toproduce the desired 75% yield pulp than are required with neutral sulfite pulp.It was apparent that the GLSC pulp had higher lignin contents at equal yields.It also appears that the GLSC and NSSC pulpsrequired essentially the same amount of refining work (Valley beater) to dropthe freeness from

500 to 200 ml CSF. Mill trials indicated that tensile and Concora strengthsof GLSC 1 5 pulps were equivalent to those of NSSC pulps, and both NSSCand GLSC pulps were lower in tensile and Concora strength thanthe corresponding laboratory produced pulps. A generaltendency for green liquor pulps was that theyrequired more beating time to lower the freeness to 500 ml CSF.Also GLSC pulps may exhibit slightly greater densities. Dawson then concluded that the GLSC hardwoodpulp was equivalent to Olinkraft's NSSC pulp in properties desirable for corrugating medium, except that the former showed a slightly lower caliperand required the use of a wetting agent on the paper machine to give desired water absorption properties.The GLSC pulp had a distinctively darker color than NSSC pulp.Corrugator trials showed the GLSC corrugating mediur . to be equal to NSSC corrugatingmedium in handling, runnability, and quality. The Virginia Fibre Corporation, at Riverville, Va. ,has carried out an experimental program to evaluate the possibilitiesof producing a high yield unbleached pine(Georgia pine) pulp by cooking with green liquor.Charbonnier, Rushton, and Schwalbe (1974) reportedthat in the pilot-plant runs, several rolls of 26-lb linerboardand 78-lb sack paper were produced withgreen-liquor pulped pine, and corrugating medium was produced with a furnish of 85%green-liquor-pulped hardwood (predominantly oak) and 15% green-liquor-pulped pine. The products were successfully converted in commercialoperation 1 6 to produce sack paper and corrugating containers, but the tearing strength of the sack paper was substantially below that for most commercial sacks. The corrugating medium had a Concora strength of 88 lb/10 flutes, and a combined board flat crush of 37.6 psi.These figures are substantially above industry averages.The runnability of the corrugating medium was classed as "reasonably good" and would be expected to improve by reducing refining. The chemical charge and cooking time were both substantially greater than with green liquor semichemical pulping of the hardwoods, and the color of all the products was rather dark brown.These draw- backs might be offset by the high yield (average of 70% or higher) and the elimination of the causticizing and lime reburning equipment which is required in the kraft recovery process. Charbonnier et al. concluded that "the green liquor pine pulps should have a place in the production of linerboard for inside liners, for use in the bottom sheet of linerboard when a secondary headbox is used,. .and for heavyweight sack paper, can stock, fiber drum stock, laminated products, etc. " The Weyerhaeuser mill at Valliant, Oklahoma, uses a wood supply consisting of 90% mixed oaks (45% red oak and 45% white oak) and 10% other mixed hardwoods for the production of corrugating medium by cooking with green liquor or blends of NSSC liquor and 1 7 green liquor.Battan, Ahiquist, and Snyder (1975) reportedthat, in laboratory experiments, the yield with 100% NSSC liquorrises considerably with the decrease in cooking temperature butwith the introduction of green liquor the effect of temperaturereduction on yield is considerably less. Concora values are not affected by the ratiosof NSSC and green liquors but are highly dependent on the pulpingtemperature for all cooking liquors, dropping sharply as the cookingtemperature is lowered below 160°C.This lost in Concora strength also takesplace even though there is,in most cases, only a slight increase inyield. The 5 min. Kappa Number values indicate that, athigher cooking temperatures, the yield loss is being affectedby cellulose being removed at a higher rate than lignin and thatlignin condensation reactions may be taking place.The pulping temperature should thus be maintained above 160°C, and170°C is preferable.Pulp yield cannot be expected to be over 72% while maintainingmaximum pulp quality. The ratio of total chemicals from the NSSC liquorand the green liquor does not significantly affect the pulpingcharacteristics of the system or the quality of the pulpproduced. The variations in sulfidity of the green liquorwill not significantly affect the pulping characteristicsof the system or the quality of the pulp produced.Increased sulfidity causes only a slight increase in the pulping rate. 18 The 5 min Kappa Number tests do not provide a good indication of pulp yield and pulp quality.Blow pH may be used as an indication to determine if the percent total chemical charge isadequate. In mill practice, actual pulping temperatures were slightlyless than those determined by research, and the cooking times weremuch longer.Total chemical charges of 8. 0-12. 0% Na20 based on o. d. wood produced good quality corrugating medium. The GLSC pulp is combined with refined kraft pulp, broke,and repulped corrugated carton clippings to produce corrugatingmedium. The resulting dark color corrugating medium hasthe same strength properties as those from NSSC pulps.

Experimental Design

The object of this project was to study the effect offive process variables, cooking temperature, chemical to wood ratio,sodium to sulfur ratio, chip size, and bark content on the pulping responseof Douglas-fir chips for production of GLSC corrugating medium. The cooking conditions and levels of variables are shown in

Table 1. Table 1.Cooking conditions.

Variables Levels

Total alkali %* )5-4- S.E- IS 'Es 1-2. t0 14 ,2 'Jr Code -2 -1 0 +1 +2 Bark % 0.0 2.5 5.0 7.5 10.0 Code -2 -1 0 +1 +2 Chip size in. (+1/16, -3/8) (+3/8 - 5/8) (+5/8 -1-1/8) Code -1 0 +1 Sulfidity % 15.0 20.0 25.0 30.0 35.0 Code -2 -1 0 +1 +2 Temperature 155.0 162.5 170.0 177.5 185.0 Code -2 -1 0 +1 +2 Liquor to wood ratio** 4:1 Heat system Steam, indirect Digester type Rotary digester Schedule Time to temperature 10-15 min. Time at temperature 60 min. Pressure variable with temperature Blow time 5 min.

Wood input Chips + Bark 5,000 grn (0.D. )/cook

*Total alkali % : (0.D. weight of total alkali (as Na20)/0. D. weight of wood) x 100. **Liquor to wood ratio: Total weight of liquor (includes water in wet wood)/total weight of wood (0. D. ). 20

The above variables were incorporated into a factorialexperi- ment as described by Cochran and Cox (1957).The plan does not include cooks at all possible levels of the factorial design.This would involve a total of 5x5x5x5x3 = 1,875 cooks, butwith the design as given by Cochran and Cox,only 30 cooks were involved.The plan is shown in Table 2. Multiple linear regression and simple linear regression pro- grams were used in this project forthe statistical analysis of the data giving the regression coefficients relating the responseof the pulp properties (such as cooking yield, physical strengths, andpH's and total solids in spent liquor) to the individual cookingvariables, as well as the interaction of the variables.This analysis can suggest optimum pulping conditions for the pulp properties,and would be valuable to those who may wish to use green liquor pulpingin commercial practice. 21

Table 2.Experimental plan. 5 x - variable N = 30 treatment combinations 1/2 replicate of 25 factorial + star design + 6 points in the center Cooking variables

Cook number* T. A. % Bark 9i, Chip size, in.Sulfidity Temp. °C X1 X2 X3 X4 X5

7 -1 -1 -1 -1 1 6 1 -1 -1 -1 -1 19 -1 1 -1 -1 -1 27 1 1 -1 -1 1 9 -1 -1 1 -1 -1 24 1 -1 1 -1 1 5 -1 1 1 -1 1 13 1 1 1 -1 -1 4 -1 -1 -1 1 -1 11 1 -1 -1 1 1 22 -1 1 -1 1 1 30 1 1 -1 1 -1 28 -1 -1 1 1 1 12 1 -1 1 1 -1 14 -1 1 1 1 -1

15 1 1 1 1 1

1 -2 0 0 0 0 16 2 0 0 0 0 26 0 -2 0 0 0 25 0 2 0 0 0 0 0 -2 * 0 0 0 0 2** 0 0 20 0 0 0 -2 0 23 0 0 0 2 0 3 0 0 0 0 -2 10 0 0 0 0 2 29*** 0 0 0 0 0 21*** 0 0 0 0 0 2*** 0 0 0 0 0 8*** 0 0 0 0 0 17*** 0 0 0 0 0 18*** 0 0 0 0 0

*Randomized order. **Only 3 levels of chip size were used in the actual experimental work as per Cochran's plan. These two experiments were thus not performed. ***Control cooks, 6 replication of the cooks in the center of the plan. 22

EXPERIMENTAL PROCEDURE

Material Flow Sheet

SECTION (I). Douglas-fir Chips Chemical Treatments Screening

Small Medium Large

Temperature °C Chemical %

Bark % Rotary Digester Sulfidity %

T. S., pH of Waste Liquor CookedChips Yield

SECTION (II). Bauer Refiner Mechanical Treatments

1 Hypochlorite Defiberated Pulp Number

1 PFI Mill

Handsheets

Physical Testing

Fig. 4.Flow sheet of materials. 23

Sample Selection

This project was part of the project "Kraft green liquorpulping of red alder and Douglas-fir for production of corrugatingmedium," which was to study wood variations and process variablesin order to provide optimum manufacturing conditions for commercialpractice for red alder as well as for Douglas-fir woods. This part of the whole project was devoted to thestudy of Douglas-fir wood.Since the bark content varies from cook tocook, it was more convenient to obtain the bark and chipsseparately.Bark- free commercial Douglas-fir chips were obtainedfrom the Western Kraft Corp. mill at Albany, Oregon, andDouglas-fir bark was obtained frotr4 Oregon State University's McDonald Forest.

Sample Preparation

Chips

Several drums of bark-free Douglas-fir chips werethoroughly blended together. A random sample of the chips wasscreened using the Williams chip classifier, and the chips wereseparated into the following fractions: +1-1/8", - 1-1/8" + 7/8", -7/8" +5/8",- 5/8" + 3/8", - 3/8" + 3/16", - 3/16" +1/16", and - 1/16".The symbol - 7/8 +5/8" means that the fraction passed through the 7/8" screen but was retained on the 5/8" screen. 24 The statistical program called for three chip sizes, - 3/8", + 3/8" - 5/8", and + 5/8" with the fine (- 1/16") andoversized (+1-1/8") chips being screened out.The well mixed chips were packed in fiber drums lined with polyethylene bags andstored in a cold room at4°C for one week to allow the moisture content to come to equilibrium. Bark from McDonald Forest was chipped and screened,and the fine (- 1/16") and oversized (+ 1-1/8") bark fractions werescreened out.The chipped bark was thoroughly mixed, andstored in a cold room similarly to the chips. Three replicate solids determinations were made onthe bark and on the three different chip fractions, and averagedto give the values used for calculating the oven dry weights ofbark and chips used in the pulping experiments. The percent solids were calculated using the followingformula:

of, Oven dry weight of chips (or bark) dried at 105 100 Solids %- Wet weight of chips (or bark)

The solids contents were checked at regularintervals to check for any possible changes in moisture. 25 Chemical Treatment

Preparation of Cooking Liquor

The synthetic green liquor for each cooking experiment was prepared according to the statistical design, as given in Table 1. Green liquor produced in a kraft mill usually contains a small amount of NaOH, because weak white liquor is sometimes used to dissolve the furnace smelt.In green liquor semi-chemical pulping, however, a causticizing step is not required, so NaOH was not used inthis Predetermined amounts of (technical grade) experiment. Na2 CO3 and a concentrated stock solution of Na2 S (technical grade) were mixed with tap water to give a final liquor to wood ratio of 4:1. The concentrations of sodium sulfide (Na2S), sodium carbonate ) and sodium hydroxide (NaOH) in the cooking liquors were (Na2 CO3 measured using the titration procedure of TAPPI Standard Method

T 624 m-60. (as 0) g/1 B = Effect alkali = NaOH + -24-Na2S Na2 = (Vol. HC1 to pH 7. 5) x (N HC1) x 6. 2 -- with BaC1 C = Active alkali = NaOH + Na2S (as Na20) g/1

= (Vol.1-1C1 to pH 7. 5) x (N HC1) x 6. 2 with BaC12 & formaldehyde 0) g/1 A = Total alkali = NaOH + Na2CO3 + Na2S (asNa2 = (Vol. HC1 to pH 4. 0) x (N HC1) x 6. 2 26

% Sulfidity = 2 ((C-B)/A) x 100 = (Na2 S/(Na2S + NaOH + Na2 CO3 )) x 100as Na20) Note:5 ml liquor sample was used for titration.

Cooking Conditions

The digester used had a rotating speed of 1/3 rpm, and was heated with either an external heat jacket or by direct steam injection. The steam flow to the digester was regulated by a Honeywell Elec- tronik 15 Cam Controller.The internal digester pressure was checked with two gages, one in the control panel and theother on the digester.The internal digester temperature was measured with a thermocouple.Because steam line condensate would change the liquor to wood ratio in the digester, direct steam injection was not used.Instead the temperature was regulated using the external heating jacket.The controller matched the thermocouple temperature with the set point temperature by changing the amount of steam enter- ing the external heat jacket. The required amount of cooking liquor and 5, 000 gm (oven dry basis) of wood (chips and bark) were loaded into the digester manu-

ally.After capping, the rotating digester was brought to temperature as quickly as possible by feeding steam intothe external heat jacket. When the proper temperature was reached, it was then controlled by the automatic cam controller. 27 At the end of the cooking cycle, the digester pressure was relieved by blowing the black liquor through a water jacketed con- denser to a container.Total weight of the black liquor was measured and samples of the black liquor were saved for further testing (pH, total alkali %, and total solids %). The chips were manually removed from the digester, and allowed to cool to room temperature by spreading them on the floor. They were then packed in polyethylene bags and stored at room temperature to allow the moisture content to come to equilibrium throughout the batch. Three samples each of 25 gm were taken from each batch, defiberated in the PFI mill, washed, dewatered, and dried to determine the solids content of the cooked chips.The averaged value was used for calculating the cooking yield (unscreened yield):

% T. S. x (total cooked chip weight (wet weight))x 100 % Cooking yield -Uncooked chip weight (oven dry weight )

Black liquor samples were analyzed for total alkali content by potentiometric titration of 5 ml of liquor with HC1:

T. A. g/1 (as Na20) = (Vol. of HC1 for pH 7 to 4) HC1) x 6. 2

The total solids content was measured for each black liquor sample using the following formula: Oven dry weight of black liquor dried at 105±3°C, 16 hr T. S. % =Wet weight of black liquor at room temperature x 100 28

Hypo Number Test

As a normal procedure, both in the laboratory and in the pulp mill, the Kappa number test is used for the determinationof the relative lignin content of the pulp, which is a valuable measureof the pulp quality.However, this test can be applied only to pulps with yields of less than 70 percent (TAPPI Standard Method T 253os-75).Batten et al.(1975) reported that the 5 min. Kappa number test does not provide a good indication of pulp yield and quality for highyield pulps. Since the yields of some of the cooks in this experimentexceeded 70 percent, the Kappa number test method cannot be relied upon. Hence, the Hypo number test, a new method for the estimationof the lignin content of high yield (relatively high lignin content) pulps, was used in this project instead of the Kappa number test. The Hypo number test method is based on the same principle of pulp treatment as the chlorine number test and measures about the same pulp properties as the Kappa number test, except that it can be applied to high yield pulps. "Pulp is reacted with acidified hypochlorite solution at25°C for ten minutes.The amount of chlorine consumed by the pulp is determined by titration and expressed as Hypo number(TAPPI,

T253 os-75). 29 Chip Disintegration

At the conclusion of the pulping operation, semi-chemical chips are still relatively hard and undefibered, because insufficient lignin has been removed to permit easy defiberization.Full chemical cooks produce relatively soft chips that break up nearly completely into individual fibers during the blowing operation, but this does not happen with semichemical cooks, and additional mechanical action is needed to defiber the chips.The chips are conventionally disintegrated in a disk refiner, such as the Bauer 187 in the Forest Research Labora- tory, following which the pulp is washed and screened.Normally the operating conditions of the disk refiner are such that the pulp has a high freeness, usually 600-700 ml CSF, in order to facilitate the washing operations, etc.Following washing, the semi-chemical pulp is further refined to lower freenesses, typically between 200 and 400 ml CSF.The final freeness desired is variable from mill to mill, and is controlled by the degree of refining in extra stages of refining that follow the chip disintegration stage. In this project, the cooked chips were disintegrated in the Bauer 187 refiner, and the plate gap was adjusted to produce pulps with freenesses between 650 and 700 ml CSF.The final pulp refining was done in the laboratory PFI mill. The cooked chips were dumped into the hopper, and were fed into the refining area with a constant flow of hot water to adjust the 30 consistency and help move the chips through the refiner. The deliberated pulps were collected and dewatered in a Bock centrifuge, packed in polyethylene bags, and stored in a cold room at 4°C to allow the moisture contents to come to equilibrium,Three samples each of 25 gm wet basis were taken from each pulp, refined in the PFI mill, washed, dewatered, and dried to determine the solids content of the defiberated pulp. The power consumption of defiberating was determined by tim- ing a known quantity of cooked chips through the refiner and obtaining a reading of energy consumption from an integrated watt-hour meter.

Pulp Refining

Semi-chemical pulps are normally given a certain amount o refining before conversion into corrugating medium, since the physical properties of the medium (burst, tensile, crush strengths, etc. ) are heavily influenced by the amount of refining and the final pulp freeness.The level of refining is variable from one mill to another, and is influenced by such factors as wood species, pulp yield (degree of delignification), and amount of recycled fiber that is mixed with the virgin pulp, to name a few.Typical commercial semi-chemical pulp freenesses are 200-400 ml CSF, and in this project each pulp was refined in the PFI mill to 200 ml CSF or below.Normally this was accomplished with 1,000 revolutions of the PFI mill. 31

For each beating interval, a sample of 24. 0 gm o.d. (calculated) disintegrated pulp was randomly takenfrom the polyethylene bags, tap water added to give a 10% consistency,and the total amount of 240 gm of wet pulp was put in the PFI mill,and beaten for the proper number of revolutions.

Handsheet Formation

With few exceptions, samples for one freenessevaluation, six handsheets at 60 gsm (gm./sq. meter) basisweight, and two corrugating medium test (GMT) handsheets at126 gsm (= 26 lb/1, 000 sq. ft) basis weight were made from each of thefour beater interval (0, 300, 650, and 1,000 revolutions) samples.Ha.ndsheets were made in ac- cordance with TAPPI Standard T205 m-58.

Handsheet Testing

The handsheets were conditioned in aTAPPI standard room at 73°F and a. relative humidity of 50% for a minimum of 48 hoursprior

to testing. For each interval, two CMT handsheets weretested in accord- ance with TAPPI StandardT809 os-71.Five of the other six handsheets were selected for physical tests,with the remaining one sheet being saved for reference purposes. Physical properties were determined in accordancewith TAPPI 32 Standard T220 m-60.An Instron TT-BLM testing machine was used for measuring the breaking length, stretch, and CMT. The testing machine was set at a crosshead speed of 1 cm/min. and the chart speed was 10 cm/min. A summary of physical test methods is given in Table 3. Table 3.Summary of physical tests.

Test TAPPI Standard Method Test Instrument Units of Measurement

Freeness T227 m-58 Canadian Standard Milliliters

Freeness Tester

Sheet density T220 m-60 Caliper Model-549 Gram per cubic centimeter

Micrometer

Breaking length T404 ts-66 Instron TT-BLM Meters

Stretch T457 m-46 Instron Percent

Stiffness T489 m-60 Taber V-5 Modulus of elasticity, lb per sq. in.

Burst factor T403 ts-63 Perkins Model C Square meters per sq. centimeter

Mullen Tester

Tear factor T414 ts-65 Elmendorf Tearing Square decimeter per sheet

Tester

Fold endurance T511 su-66 MIT Fold Tester Number of double folds

Corrugating medium T809 os-71 Instron TT-BLM lb per 10 flutes

test (Concora) 34

RESULTS AND DISCUSSION

Sample Preparation

A random sample of the bark-free Douglas-fir chips was screened using the Williams chip classifier, and in Table 4, the chip size distribution of this sample is given.

Table 4.Size classification of Douglas-fir chips. Chip size Screen fraction (%)

+ 1-1/8" 3. 3 1-1/8" +7/8" 6. 3 7/8"+ 5/8" 19. 3 5/8/1,+ 3/8" 41. 9 3/8"+ 3/16" 24. 6 3/1611 + 1/16" 4. 2 1/16" O. 4 Total 100.0

The statistical program called for three chip sizes, - 3/8", + 3/8" - 5/8", and + 5/8" with the fine (- 1/16") and oversized (+ 1-1/8") chips being screened out.

Pulping Results

The multiple regression analysis, multiple regression equations, effect of independent variables, and predicted maximum value 35 and maximum value conditions of cooking variables (totalalkali %, chip size, sulfidity %, bark %, and temperature) on pulping results (total solids in waste liquor, pH value of waste liquor, and pulp yield) are given in Tables 5 and 6.

Total Solids in Waste Liquor

From Table 5R2= 0. 891, F value 7- 5. 483, indicated thatthe total solids in waste liquor (T. S. W. L. ) are highly correlated to the cooking variables at the 0. 05 significance level.Table 5 revealed that the total alkali (T. A. )(-h) had the most effect on total solids in waste liquor at the 0. 01 significance level, and the cooking temperature also had some effect on the total solids in waste liquor. Table 6 shows that at high LA., high temperature, high bark, high sulfidity, and large chip size, T. S. W. L. has the maximumvalue

of 1, 583 g.

pH Value of Waste Liquor

From Table 5 78% of the pH value of waste liquor can be explained by the multiple regression analysis (not significant).Table 5 indicates that the T. A. and temperature are the most important variables.The pH value is of importance to the pulp mill only as a cri- terion of the consumption of the cooking chemicals, and there is no significance attached to its maximization. Table 5.Multiple regression of cooking variables to pulping results. Variables d. f. -F value T. S. in waste liquor, g.pH value in waste liquor Yield % Total terms 20 5.483 ( 0. 05)t(a) 1.840 2. 920 (0.25) First order termsl 5 4.708 6.508 1.717 Second order terms 15 1.993 0.835 1.420 Lack of fit 4 2.123 1. 274 1. 583 R oz, total terms 0. 891 0.783 0. 838 Error( mealuguare) x102 5 49.3 15. 1 5. 6 T. A. 0A* 14.96 (0.005) 4.01 (0. 10) 3. 05 (0. 25) Bark %** 0.19 0.50 2. 33 (0. 25) Chip size 71*** 0.66 0.62 2. 39 (-0. 25) Sulfidity %**** 0.67 0.95 1.09 Temperature°C***** 1.46 1.32 1.53

Note: 1. First order terms = X( 1 )+... +X(5). Second order terms = X(6)+... +X(20). o X(1) = T. A. %, X(2) = Bark %, X( 3) = Chip size, X(4) = Sulfidity %, X( 5) = Temperature X(6)= X(1)2, X(7) = X(2)2, X(8)=X(3)2, X(9)= X(4)2, X(10)= X(5)2; = X(1) x X(2), = 1) x X(3),

X(3) x X(5), = X(4) x X(5). The complete effects of Total alkali %, Bark %, , Temperature (as asingle first order term and five second order terms) were listed by deleting the six appropriate variables from thefull response surface model. X(1), X(6), X( 11), X(12), X(13), and X(14) were deleted. ** X(2), X(7), X(11), X(15), X(16), and X(17) were deleted. *** X(3), X(8), X(12), X(15), X(18), and X(20) were deleted. *4** X(4), X(9), X 13), X(16), X(18), and X(20) were deleted. ***** X( 5), X( 10), X(14), X( 17), X( 19), and X( 20) were deleted. ( a), significance level. Table .6.Predicted maximum value of pulping results. Pulping results Maximum value conditions Y, predicted maximum X( 1) X(2) X (3) X(4) X(5) value

T. S. in waste liquor, g +2 +1 1583.1 pH value in waste liquor 0 -2 -1 -2 -2 9.83

Pulping yield, % -2 -2 -2 91.64

Note:X(1) = total alkali %. = bark content %. = chip size,". = Sulfidity %. = Temperature

Three levels (-2, 0, and +2) of each of the five cooking variables were chosen to find out the predicted maximum value and maximum value conditions, by using the multiple regression analysis equations which are given in Appendix Table 1. 38 Pulp Yield

From Table 5 pulp yields are highly correlated tothe cooking variable(R2=0.84), and Table 5 indicates that the T. A. (-) is the most important variable. Table 6 shows that lower T. A. ,lower temperature, lower bark content, higher sulfidity, and larger chip size,result in the maximum

pulp yield value.With the possible exception of the sulfidityvariable, these other effects are consistent with generallyaccepted principles of pulping, i. e.mild conditions produce pulps with high yields. A simple linear regression related T. S. W. L. topulp yield with

R2= 0. 19, at the 0. 025 significancelevel.

Hypo Number Test

Most unbleached pulps are routinely tested for lignin content in commercial operations.The Klason lignin test is tedious and lengthy, and alternative methods of estimating lignin contenthave

been devised.Most of these tests are based on oxidation of thelignin by specific chemicals such as KmnO4 (potassium permanganate -the K number, or alternatively, the Kappa number test), orby various chlorine compounds such as NaC10, sodiumhypochlorite.The K no. or Kappa no. test works best withfull chemical pulps that are well delignified (about 50% pulp yield) but lacks precisionand accuracy 39 with semi-chemical pulps that are incompletely delignified (60% yield and higher).Recent developments have suggested that oxidation with NaC10 is a good method of estimating the lignin contentof semi- chemical pulps with precision and accuracy, and it wasexamined in this project for its utility. Since the precision of yield determination for the controlcooks was poor, it was decided to test thesepulps first to see if there was a good correlation between theyield and the hypo numbers of the six different pulps (Table 7).Theoretically they should be positively correlated. A casual examination a the data suggests poorcorrela- tion, and this is verified by ther2of the linear regression, 0. 02. Particularly disturbing is the fact that the hypo numbersof the highest yield cook (no. 27) and the lowest yield cook no14) are identical, in spite of the difference in yield of 13%. Examination of the pulps revealed that the highyield pulp, cook

no.27, had a large percentage of shives, or fiberbundles, compared

to the low yield pulp, cook no.14.Past research work has estab- lished that one of the reasons for the poor precision and accuracy a the Kappa number test, in the high yield region, isthe presence of large amounts of shives.The oxidizing chemical does not pene- trate the shives as readily as it penetrates dispersedfibers, and so the chemical consumption for a high yield pulp is not as great asit should be. Table 7.Hypo number test.

Cook No. 2* 8* 17* 18* 21* 29* 27 14

Yield % 70.17 71.36 70.01 70.41 67.34 67.75 78.75 65.52 PFI revolutions 300 300 300 300 300 300 300 300 Sample weight 0.4790 0.5437 0.5631 0.4594 0.4849 0.4936 0.4843 0.4318 (o.d.g ) 0.3923 0.4589 Hypo no. 39.19 30.12 31.39 31.18 29.68 28,42 29.86 29.85 29.41 29.44

* Control cooks Three samples of control cook no. 2 were tested to determine the variability of this test. Dried handsheets were disintegrated and used as test specimens. Sample weight 0.5 gm (o. d. ). r2= 0.02 for linear regression, hypo number vs. yield. 41

To see if this phenomenon had any effect onthe results of the hypo test, samples of cook no. 27 were disintegratedfor 600 and 900 revolutions in the PFI mill, and duplicate hypo numbertests were performed for each sample (Table 8).From this data, it appeared that the hypo value passes through a maximum at600 revolutions which did not seem reasonable.

Table 8.Hypo number vs. beating revolution (PFI).

Cook no. Revolution Sample weight (o.d. g ) Hypo no.

600 0.470 33.92

600 0.502 34.18 27 900 0.455 3.50

900 0. 536 32. 31

Note: At each revolution level two samples were tested.Dried handsheets (dry samples) were used as test specimens.

Another factor which was checked was theinitial pulp condition. If dried pulp is used for the test,it may be very difficult to defiber the samples completely, since some of thedried pulp is very tenaci-

ously bonded.Then the same difficulty may be encounteredin the hypo (or Kappa) test, as with the shives inpoorly defibered pulp. To test this, a series of hypo number tests were runon wet pulp, never dried, prepared at 300,600, and 900 PFI revolutions (Table 9). The first three values are essentially equal, butthe last value, 32. 86, is much higher.Since this sample weight was much higher, it 42 appeared that sample weight may affect the hypo test.The standard method does not specify a certain amount of pulp, but suggests ranges of sample weights for different grades of pulp.

Table 9.Hypo number vs. beating revolution (PFI).

Cook no. Revolution Sample weight (o. d. g ) Hypo no.

300 0. 483 30. 30 27 600 0. 277 30. 50

900 0. 236 30. 69 27 900 0. 420 32, 86

Note: Wet pulps (wet samples) were used.

Table 9-1. Hypo number vs. beating revolution ( PFI).

Cook no. Revolution Sample weight (o. d. g) Hypo no.

300 0.483 30,30

27 600 0.502 31.66

900 0.420 32.86

Note: Wet pulps (wet samples) were used.

Table 9-1 presents the hypo numbers (at substantially equal sample weight) for pulps refined for 300, 600, and 900 revolutions in the PFI mill, and the hypo number is nearly linear with PFI revolutions. The work was not pursued further, due to some of the discrep- ancies found in the test procedure, but the following recommendations 43 are made for future work with semi-chemical pulps: Use a constant amount (dry basis) of wet, never dried pulp for testing. Defiber the pulp completely to a constant degree, either measured by the amount of refining (as in the PFI mill), or by refining to a constant freeness.

Chip Disintegration and Pulp Refining

Clearance Determination

Control cook no's 18 and 2 were used for determining the Bauer plate clearance necessary to give a defiberated pulp freeness level of 650-700 ml CSF.The disintegration data are shown in Table 10.

Table 10.Disintegration data.(Bauer refiner.

Cook no. Plate clearance, Output freeness, Power consumption, mils ml. CSF hp-clay/ o. d. ton

18 20 640

18 30 743 average28. 8

18 40 759

8 25 677 24.2

Note:Single pass. Steam at throat screw. Refining speed.1, 755 rpm. Stock at room temperature 70°F. Constant water flow, 1 gal/min.

Based on this work, a Bauer plate clearance of 25 mils was selected for disintegration of the remaining batches of cooked chips. 44 Power Consumption and Initial Freeness

The importance of refiner clearance to the drainage properties of the pulp was demonstrated when smaller clearances were inadver- tently used to refine cook no. 's 17, 21, and 29.The pulps obtained had low freenesses, and the power consumptions were higher than average (Table 11).

Table 11.Power consumption.

Cook no. Output freeness, Power consumption, ml. CSF hp - day/o.d. ton

745 26.3

8 677 25.3

17 512 76.7

18 743 28.8

21 626 42.6

29 701 57.5

Note: Control cooks only.

The initial freeness of the pulp following the Bauer refiner is a measure of the amount of disintegration work done by the Bauer refiner.In order to find out the effect of disintegration work on pulp properties, initial freeness was sometimes treated as an independent varia.lbe along with the cooking variables in the multiple regression analysis. Linear regression analysis of the power consumption vs. initial 45 freeness suggests good correlation(R2=0.62, F=45.66, significance level = 0. 01, sign of B = (-) ) (Appendix Table 1).

PFI Refiner

It was necessary to establish, by trial and error, the proper number of revolutions needed to refine the various pulps to 200 ml CSF or below.Control cooks no. 's 8 and 29 were used to determine the PFI revolutions, as shown in Table 12.

Table 12.Refining data. (PFI mill)

Cook no. Input pulp freeness, PFI Output pulp freeness, ml. CSF revolution ml. CSF

0 677 300 515 677 650 359 1,000 195

0 701 300 604 29 701 650 333 1,000 210

Since the freenesses at 1, 000 revolutions, 195 and 210 ml CSF, were on target,. four beating intervals of 0, 300,650 and 1, 000 revolutions, were chosen for further refining experiments. 46

Pulp Quality

Introduction

Normal production specifications call for a commercial grade corrugating medium with a bulk of 1. 8 cc/gm (26 lb/1, 000 sq ft basis weight and a caliper of 9 mils (0. 009 in)).In this project pulps with freenesses of 200 ml CSF or below were needed to meet this requirement, and they required 1, 000 or more PFI revolutions to attain this freeness level. Since nearly all paper properties are functions of the basic sheet density (or its reciprocal, bulk) which in turn is a function of the amount of refining, the strength properties of the 30 different pulps were compared on three separate bases: Constant bulk (1. 8 cc/gm). Constant freeness (200 ml CSF). Constant PFI revolutions (1 000 revolutions). They could be compared at other levels (such as 600 and 400 ml CSF for constant freeness) but the levels given above are the closest to the values of pulp properties and process variables that are consistent with the production specifications already given. The correlation of the ha,ndsheet properties to the independent cooking variables, the effect of each independent variable on handsheet properties, and the maximized handsheet strength properties 47 are given in Tables 13, 14, and AppendixTables 3, 4,5, and

Concora Strength

Concora strength, as expressed in lbs/10 flutes, is oneof the most important pulp properties of corrugating medium.

200 ml CSF: The analysis shows that at the 0. 05 significance level, only 53% of the Concora strength can be explained by themultiple regression analysis.From Table 13, the bark content (-), total alkali (-), and percent sulfidity (+) were significantlycorrelated to the Concora strength at the 0. 05 level.

The simple linear regression table (Appendix Table1) indicates that at the 0. 01 significance level, PFIrevolutions are related to the Concora strength withR2= 0. 4. 1, 000 PFI revolutions level: The F value analysis indicates that none of the cooking variables had a. significant effect on the Concora strengths

(R2=0. 56,not significant). The predicted maximum value of 86 lb/10 flutes was obtained at exactly the same conditions as in 200 ml CSF level. With the addition of initial freeness as one of the inde-

pendent variables, theR2value increases from 0. 56 to 0. 75, indicating that the Con.cora strength is influenced bythe initial Table 13.Multiple regression of cooking variables to Concurs stren

Variables d. f. F value 200 ml CSF 1,000 Revs. 1. 8 Bulk 0 Revs.

Total terms 20 4. 34 (0.10)(a) 0.66 3.43 (O. 10) 0.16 First order terms 5 7.61 1.31 2.61 Second order terms 15 5. 12 0.59 3. 76 0.17 Lack of fit 4 17.52 1.75 11. 18

2 0. 533 0.560 0. 579 0.406

Error (mean square) 5 7.10 29.4 15.8 7. 35

0.16 T. A. % 4. 69 (0. 10) 0.66 4. 34 (0. 10)

Bark 5. 48 (0. 05) 0.73 4. 64 (0. 10) 0.21 Chip size n 3. 05 (0.25) 0.53 5. 51 (0. 05) 0.09 0.13 Sulfidity % 6.48 (0.05) 0.69 7.03 (0. 025) Temperature °C 3. 36 (0.10) 0.90 5. 38 (0.05) 0.08

Note:in "-", the value was less than 0. (a), significance level. 49

freeness of the pulp (1. e. , amount of Bauer refiner work).

(3)1. 8 Bulk level: Table 13 indicates that the sulfidity (-) is the most important individual cooking variable, at the 0. 025 significance level, chip size (+) and temperature (-) also contributed significantly to the Concora strength at the 0. 05 significance level.Total alkali and bark content also affected the Concora strength. As opposed to the results of the 200 ml CSF and 1, 000 PFI revolutions levels, the maximum value conditions show that Lower sulfidity and larger chip size gives the maximum Concora strength value of 80 lb/10 flutes. Again, the simple linear regression table (Appendix Table 1) indicates that at the 0. 01 significance level, the PFI revolutions are related to the Concora strength withR2= 0. 56,

The Concora test is not a simple test, with many chances for experimental errors.Variations in handsheet preparation, in fluting or corrugating produces (pressure and temperature), and infinal assembly and testing of the samples can result in substantial devia- tions of the final test results.This may be a partial explanation of the lack of correlation between Concora and other variables. 50 Tensile Strength

200 ml CSF The tensile strength is highly correlated to the first and second order terms of the cooking variables(R2=0.922), at the 0. 025 significance level (F=7. 56). In the full regression equation, the total alkali (+) is the most important variable (F=15. 9, at the 0. 005 significance level), and chip size (-) and sulfidity (+) are also significantly correlated to the tensile strength at the 0. 05 and 0. 10 significance level, respectively. Table 14 shows that at higher total alkali, higher sulfidity, higher temperature, lower bark content, and small chip size, the tensile strength has the maximum value. The predicted maximum value of 18,757 meters is much too high, but is caused by the multiple regression maximum value approach.However, the conditions for the predicted maximum values can be treated as guidelines to obtain the maximum practical level of the particular property. 1,000 PFI revolutions The multiple regression analysis indicates that the tensile strength is highly related to the cooking variables, with theR2 equal to 0.857.The total alkali (+) is the most important Table 14.Predicted maximum value of pulp properties. Pulp Properties Level Maximum value conditions Predicted maximum value, X(1 ) X(2) X(3) X(4) X(5) 200 ml CSF -2 -2 -1 +2 -2 100.4 1,000 revs. -2 -2 -1 +2 -2 86.4 Concora strength 1.8 Bulk +2 +2 0 -2 +2 82,0 (-2 -2 +1 -2 -2)* 80.0 0 revs. 0 0 0 0 0 15.3

200 ml CSF +2 +2 -1 +2 -2 18, 757. 9 (+2 -2 -1 +2 +2)** 16, 350.0 1,000 revs. +2 -2 -1 +2 +2 17, 763. 5 Breaking length 1.8 Bulk +2 -2 -1 +2 +2 21, 048. 3 0 revs. +2 -2 -1 +2 +2 6, 548. 3

200 ml CSF +2 0 0 +2 -2 43,24 1,000 revs. +2 0 0 +2 -2 41.40 +2 0 -1 +2 0 51.20 Burst factor 1.8 Bulk 0 0 +2 0 \ 49.00 +2 0 -1 +2 +2 )**) 49. 00 (+2+ 2 0 -1 +2 _2J 47.00 0 revs. +2 -2 +2 0 10. 00

Note:X(1) = total alkali %. X(2) = bark content %. X(3) = chip size ". X(4) = sulfidity %. X(5) = temperature °C. *The next higher value of Concora strength at 1. 8 bulk. **The next higher value of Breaking length at 200 ml CSF. 4**The next higher value of Burst factor at 1.8 bulk. 52 variable in the full regression equation, at the 0. 05 significance level. Table 14 indicates that higher total alkali, higher sulfidity, higher temperature, lower bark content, and small chip size (the same conditions as in 200 ml CSF level) produce the maximum tensile strength.Again, the maximum predicted maximum value is somewhere beyond the normal range of tensile strengths. With the addition of initial freeness as one of the independent variables, theR2value increases from 0. 857 to 0. 926, indicating that the tensile strength is influenced by the initial freeness of the pulp (i. e, amount of Bauer refiner work).

1. 8 Bulk Table 15 shows that the total alkali (+) is the most important variable, at the 0. 05 significance level.Chip size (-) and sulfidity (+) also have some effect on the tensile strength. Table 14 gives the same maximum value conditions as for the 200 ml CSF and 1, 000 PFI revolutions levels.Once again the predicted maximum value is beyond the practical range. 0 PFI revolutions Eighty-four percent of the variation of tensile strength of the unbeaten pulp can be explained by the multiple regression analysis (F=1. 8, not significant).The analysis reveals that 53 total alkali has a significant effect on tensilestrength, at the 0. 10 significance level. Table 14 indicates exactly the same conditionsfor maximum tensile strength as thosefor the 200 ml CSF, 1, 000 PFI revolutions,1. 8 Bulk, analysis, with a maximumtensile strength of 6, 550 meters.This is a reasonable value.

In all cases (ZOO ml CSF, 1, 000 PFIrevolutions, 1. 8 Bulk, and PFI revolutions), the independent pulpingvariables show the same type of influence on the tensilestrengths of the pulps, lower bark content and lower yield both are importantin promoting high tensile strength, and the low yield can beobtained in a variety of ways of adjusting the pulping conditions.

Bursting Strength

(1) 200 ml CSF The high R2 value (Table 16) indicatesthat 95 percent of the bursting strength can be explainedby the first and second order terms of cooking variables, at the 0. 05significance level. The analysis shows that both total alkali(+) and sulfidity (+) are the most important variables in the fullregression equation, at the 0. 01 a. ncl 0. 05 significance levels,respectively. Table 14 shows that at higher total alkali,higher sulfidity, lower temperature, medium chip size,and medium bark Table 15.Multiple regression of cooking variables to Breaking length.

Variables d. f. F value 200 ml CSF 1,000 Revs. 1.8 Bulk 0 Revs.

Total terms 20 7..56 (0.025)(a) 2.40 (0.25) 2.40 (0.25) 1.82 First order terms 5 0.67 0.36 0.65 0.93 Second order terms 15 4.50 1.43 1.47 1.36 Lack of fit 4 1.32

2 0.922 0.857 0.840 0.831 5 Error (mean square) x 10 5 6.78 23.5 29.9 4.63

T. A. % 15.90 (0.005) 4,, 98 (0.05) 4.94 (0.10) 3.48 (0.10)

Bark % 3.06 (0.10) 0.96 0.60 1.35 Chip size If 5.92 (0.05) 2.14 (0.25) 3.08 (0.25) 1.81

Sulficlity % 4.86 (0.10) 1.92 (0.25) 1.98 (0.25) 1.28 Temperature oC 3.81 (0.10) 1.01 0.59 0.71

Note:in 'L.", the value was less than 0.1. (a), significance level. Table 16.Multiple regression of cooking variables to Burst factor.

Variables d. f. F value 200 nil CSF 1,000 Revs. 1.8 Bulk 0 Revs.

1.13 Total terms 20 9.54(0.025)(a) 71.39 (0.005) 9.01 (0.025) First order terms 5 4.12 2.67 3.28 1.03 Second order terms 15 2.01 3.33 2.65 0.88 Lack of fit 4 1.12 16.99 2.86

2 0.953 0.954 0.840 0.831

Error ( mean square) 5 6.17 9.10 8.00 4.36

1.85 1.61 T. A. % 19.1310.005) 13.42 (0.01) 1.22 Bark % 1.62 1.85 0.25 Chip size 0.42 0.53 0.23 0.76 0.44 0.50 Sulfidity % 9.19 (0.025) 6.69 (0.05) Temperature °C 2.-67 (0.25) 1.93 (0.25) 0.28 0.32

Note:in "-", the value was less than 0.1. (a), significance level. 56 content, the burst factor has the maximum value of 43M2/cm2. This is a reasonable value. 1, 000 PFI revolutions The bursting strength is highly related to the cooking variables(R2=0.954F=71.4, significant at the 0. 005 level). The analysis indicates that total alkali (+) and sulfidity (+) are the most important variables, significant at the 0. 01 and 0. 05 levels, respectively. The predicted maximum value of 41M2 /cmis given as a function of the same conditions asthose at the 200 ml CSF level (high total alkali, high sulfidity, low temperature, medium chip size, and medium bark content). 1. 8 Bulk Compared to the 200 ml CSF and 1, 000 PFI revolutions levels, the bursting strengths at 1. 8 cc/gm bulk level have an

R2of 0. 84, and F = 9.01 which is significant at the 0. 025 level. Again, both total alkali (+) and sulfidity (+) are the most important variables in the multiple regression analysis, significant at the 0. 01 and 0. 05 levels, respectively. Table 14 indicates that either medium chip size and medium temperature, or minimum chip size and maxim.um temperature produce the maximum bursting strength, withthe other variables constant.Generally those factors are those which 57 produce low yield pulps. (4) 0 PFI revolutions

The analysis(R2=0.831, F=1. 1, not significant) indicates that none of the cooking variables is significantly related to the bursting strength.

Tearing Strength

TheR2values ranged from 0. 69 at the 1. 8 cc/gm bulk level to 0.86 at the 0 PFI revolutions level, but the smaller F values (Table 17) shows that the cooking variables are not significantly correlated to the tearing strength. Table 17 indicates that, at the 1, 000 PFI revolutions level, both sulfidity (+) and temperature (+) are the most important variables, significant at the 0. 25 level, but at the 0 PFI revolutions level, total alkali (+) and bark content (+) turn out to be the most important variables, both significant at the 0. 25 level. However, Table 17-1 indicates that the maximum value conditions are identical for all four levels,i. e. ,at higher total alkali, higher sulfidity, higher temperature, higher bark content, and smaller chip size, the tearing strength has the maximum value.

Stiffness, (M0)

The multiple regression analysis suggests that the significance Table 17.Multiple regression of cooking variables to Tear factor.

Variables d. f. F value 200 ml CSF 1, 000 Revs. 1.8 Bulk 0 Revs.

Total terms 20 0.90 1.66 0.59 2. 15 (O. 25)(a) First order terms 5 0.53 1.27 0.64 0.98 Second order terms 15 0.60 1.83 0.56 1.43 Lack of fit 4 --

2 0.729 0.833 0.687 0,863 Error ( mean square) xio2 4.77 2.82 1.36 4.39

T. A. 0.16 0.94 0.29 2. 89 (0. 25)

Bark 0.27 0.74 0.72 2.04 (0. 25) Chip size 0.25 0.90 0.38 1.10 Sullidity 1.36 2. 32 ( 0.25) 0,62 0.82 Temperature oC 0.20 2. 18 ( 0, 25) 0,80 0.89

Note:" value less than 0. 1. ( a), significance level. Table 17-1.Predicted maximum value of pulp properties. Pulp Properties Level Maximum value conditions Predicted maximum value, X(1) X(2) X(3) X(4) X(5)

200 ml CSF +2 +2 -1 +2 +2 234 1,000 revs. +2 +2 -1 +2 +2 281 Tear factor 1.8 Bulk +2 +2 -1 +2 +2 386 0 revs. +2 0 -1 +2 0 177

200 ml CSF +2 -2 +1 +2 -2 700, 395 1,000 revs. +2 -2 +1 +2 -2 663,834 +2 -2 0 +2 -2 505,603 Stiffness, MOE 1.8 Bulk +2 -2 +1 +2 -2 486,000 (+2 -2 -1 +2 -2) 498,000 0 revs. +2 -2 -1 +2 -2 152,178

200 ml CSF +2 -2 -1 0 -2 0.91 Bulk 1,000 revs. +2 -2 -1 +2 -2 1.17 0 revs. +2 +2 -1 +2 +2 6.11

1,000 revs. +2 +2 0 -2 -2 644 Freeness, ml CSF 1.8 Bulk -2 -2 +1 +2 +2 793 0 revs. -2 -2 +1 -2 -2 948

PFI revolutions 200 ml CSF -2 -2 +1 -2 -2 2,528 100 x log revs. 1.8 Bulk -2 -2 +1 -2 -2 814 60 of correlation between cooking conditions and stiffness is minimal for three out of four bases of comparison. Only at the 1. 8 cc/gm bulk level(R2=0.63, F=2. 19 significant at the 0. 25 level) is there any reasonable degree of correlation. Table 18 indicates that at the 1. 8 cc/gm bulk level, sulfidity(+), total alkali (+), and bark content (-) are significant at the 0. 25 level. The maximum value conditions indicates that, at lowerfreeness levels,if other cooking conditions are kept constant, pulp from large chips has higher stiffness than pulp from small chips.Otherwise, at the higher freeness level pulp from small chips has the higher value.

Freeness, Bulk, and PFI Revolutions

Freeness (ml CSF) is calculated at specific levels of bulk and beating revolutions; bulk (c /g) is calculated at specific levels of freeness and beating revolutions; and the number of beating revolutions (in PFI mill) is calculated at specific levels of freenessand bulk.For each of the three properties independently, Tables 19, 20, and 21 show that the cooking variables have no significant effect on these properties (low F value), and none of the individual cooking variables has a significant effect on both freeness and bulk, atall levels. Tables 17-1 and 21 indicates that at the 1. 8 cc/gm bulk level, total alkali (-) and sulfidity (-) significantly affect the PFIrevolutions, Table 18.Multiple regression of cooking variables to Stiffness (MOE).

Variables d. F value 200 ml CSF 1,000 Revs. 1. 8 Bulk 0 Revs.

Total terms 20 1.09 0.83 2. 19 (0.25)(a) 0.73 First order terms 5 0. 81 0.48 0. 97 0. 85 Second order terms 15 0.79 0. 54 1.77 0.72 Lack of fit 4 5. 18

R2 0.868 0.732 0. 630 0.734 Error ( mean square) x108 5 29.1 31. 3 8.59 6.55 _

T. A. 0.95 0.79 1.50 1.48

Bark % 1. 15 1. 09 1. 97 (0. 25) 1. 03 Chip size 0.73 0.48 1. 67 1. 25 2. 46 (O. 25) 0.91 Sulfidity % 1.28 1.04 Temperature oC 0.88 0.63 2. 31 (0. 25) 0.96

Note:in places of 1,-", the value was less than 0. 1. (a),Significance level. Table 19.Multiple regression of cooking variables to Freeness, ml CSF.

Variables d. f. F value 200 ml CSF 1, 000 Revs. 1. 8 Bulk 0 Revs.

Total terms 20 0.50 1.17 0.14 First order terms 5 1.12 0.97 Second order terms 15 5.93 1.15 0.16 Lack of fit 4

2 0.577 0.737 0. 734 3 Error (mean square) x 10 5.81 10.6 7.51

TA. 0.36 1.33 0. 11 0.21 Bark 0.65 0.92 Chip size 0.41 1.75 0.13 0.05 Sulfidity 0.92 0.87 0.12 Temperature oC 2.76 0.S1

Note: "-" value less than O. 1. Table 20.Multiple regression of cooking variables to 3u1k.

Variables d. f. F value 200 ml CSF 1,000 Revs. 1.8 Bulk 0 Revs.

Total terms 20 0.48 0. 53 0.83

First order terms 5 0. 39 0. 54 0.87

Second order terms 15 0.45 0.47 0.70 Lack of fit 4

2 0.653 0.674 O. 732 Error (mean square)10-2 8.68 6.98 26. 2

T. A. % 0.59 0.45 0.91

Bark % 0. 39 0.48 0.78 Chip size 0. 24 0. 28' 1.10

Sulfidity % 0. 33 0. 64 0.37 Temperature °C 0. 62 0. 62 0.99

Note:'Li, value less than 0. 1. Table 21.Multiple regression of cooking variables to PFI revs.

Variables d. f. F value 200 ml CSF 1,000 Revs. 1.8 Bulk 0 Revs.

Total terms 20 0.46 2.20#

First order terms 5 0.98 3.78# Second order terms 15 0.51 -- 2.29# Lack of fit 4 0.71 3.03#

2 0.52 0,720# 3 Error mean sware x 10 5 107.0 2.01#

T. A. 0.16 2.01#( 0.25)(a)

Bark 0.27 0.76# Chip size 0.25 1.51# Sulfidity 1.35 3.52# ( 0.10) Temperature Oc 0.20 0.96#

Note: "#" at log revs. x 100 level (a), significance level. 65 at the 0. 25 and 0. 10 levels, respectively. Table 17-1 shows a trend that the pulps with high yield need more refining work to reach the same freeness level than pulps with lower yield.It also appears that pulp at the 1. 8 cc/gm level is at a lower freenesii level than pulp beaten with 1,000 PFI revolutions.

Stiffness and Concora Strength

The flat crush test of corrugating medium (Concora strength) is time-consuming and results are subject to numerous operating errors, since it is dependent not only on the sample of corrugating medium but also on the quality of adhesive tape used and the condition of the corrugator, to name a few factors.Moreover, the skill of the operator very significantly affects the strength of the corrugated medium. If a simpler and more precise test could be developed for pre- dicting corrugating medium performance, it might be a worthwhile contribution to industrial practice. Theoretically, stiffness (MOE) and flat crush tests are measuring the same property of paper, namely rigidity.The flat crush test measures the resistance of a fluted paper structure to a load applied normal to the flutes, but the Taber machine measures the stiffness (MOE) of a flat sheet ]of paper by measuring the resistance of the sheet to a bending stress.It is a simple, rapid test using a device 66 that is readily calibrated and reasonably foul proof, and thus meets some of the criteria for a good test method. A linear regression analysis was run for each cook, using the M0E's (X's) and Concora strengths (Y's) at the 0, 333, 666, and 1,000 revolutions PFI beating intervals, with good results.The

averageR2for the 30 cooks was 0.90, with 0. 99 as the highest and 0.71 as the lowest.Pooling all the data (120 sets = 30 cooks x 4 intervals per cook) in one regression, the overallR2= 0. 74, with an F = 335, significant at the 0. 001 level. These calculations show excellent correlation between the two tests overallWhether the Taber stiffness test (for MOE) could be used commercially to supplement the Concora test is not known, but it appears to be a good possibility.

Comparison of Different Semi-Chemical Pulps

GLSC and NSSC Softwood

The comparison of GLSC and NSSC softwood corrugating medium is shown in Table 22.

GLSC and NSSC Hardwood

The comparison of GLSC and NSSC hardwood corrugating medium is shown in Table 23. Table 22.Comparison of GLSC and NSSC softwood corrugating medium-handsheet data. Georgia pine* Douglas-fir Cooking liquor 100% GL 100% NS** 60°/NS + 40% GL*** 100% GL **** Total alkali % 17.2 6.0 6.0 SrA 6.0 tE-re to.0 Yield, % 72. 8 77. 3 72. 3 73. 5 70. 3

Freeness, ml CSF 500 400 400 400 200 400 Burst factor,(its,42ern2) 49 17 20 24 Tear factor, (din /sheet) 183 --- 123 96 145 Breaking length, (meter) 4, 761 5, 520 5, 000 4, 670 5, 372 5, 739 Concora, (lb/10 flutes) --- 51 39 36 48 39

* Data from Charbonnier, Ruston, and Schwalbe (1974). ** Data from Bublitz (1973), unpublished private data, Forestry Research Laboratory, Oregon State University. *4044 Data from Bublitz (1973); Blended cooking liquor with 60% neutral sulfite liquor and 40% kraft green liquor. **4c* Each value is average of 7 sample values, under similar cooking conditions. Comments The chemical charge for GLSC Douglas-fir chips was substantially less than that used with Georgia pine to reach the same yield level. Under similar pulping conditions, kraft green liquor is a faster pulping material than neutral sulfite pink liquor (Bublitz(1973)).The yields of Douglas-fir GLSCpulps are lower than those of NSSC Douglas - fir pulps. At the 400 ml CSF level, the Concora crush strength of GLSC Douglas-fir corrugating medium is lower than that of NSSCDouglas-fir corrugating medium. On the same yield basis, GLSC Douglas-fir pulp has lower tearing and bursting strength than Georgia pine GLSCpulps. Tensile strengths of the GLSC Douglas-fir pulp tend to increase with decreasing yield, and are about the same orslightly higher than those of GLSC Georgia pulps.. Table 23.Comparison of GLSC and NSSC hardwood corrugating medium - handsheet data. Western oak (1) Midwestern (Z) Midwestern (3) Douglas-fir (4) 90% oak + 10% other hardwood Cooking liquor 100% NS 60% NS + 40% 100% GL 100% NS 100% GL

Total alkali % 8.0 12.0 16.0 8.9 43149 6.0 .71.4."/ 1-214 t 47, 0 Pitre.12, Yield % 66. 0 70. 8 70.8 76. 8 73.5 70. 3 69. 9

Freeness, ml CSF 400 300 r 300 300 200 300 300 300 Breaking length, (meter) 3,730 3, 839 3, 840 4, 670 5,021 6, 308 5, 032 Burst factor, (m2/ cm2 ) 21 24 20 17 26 24 Concora strength, (11)/10 flutes) 65 51 50 68 48 42 43 42 Data from Bublitz (1974). Data from Battan, Ahlquist and Snyder (1975.). Data from Dawson (1974). Each value is average of 7 sample values, under similar cooking conditions. Blended cooking liquor of 40% green liquor and 60% neutral sulfite pink liquor. Blended cooking liquor of 60% green liquor and 40% neutral sulfite pink liquor. Comments At the 400 ml CSF level, GLSC Douglas-fir pulp has lower Concora strength than GLSC and NSSC hardwoodpulps.Generally speaking, hardwoods have been preferred to softwoods for corrugating medium because of their short fibers, which improvethe sheet structure and stiffness, resulting in higher Concora strength. Under similar cooking condition, GLSC Douglas-fir pulp has about the same yields as GLSC and blended GLSC + NSSChardwood pulps (midwestern oak).The pulp yield is substantially higher than that of western oak NSSC pulp. At equivalent levels of yield, freeness, or chemical charge, GLSC Douglas-fir pulp has higher tensilestrength than GLSC and NSSC hardwood (western and midwestern) pulps. The bursting strength of GLSC Douglas-fir pulp is about the same as the GLSC hardwood pulp bursting strength. Since the Concora strength of Douglas-fir pulp tends to increase with increasing refining work, the GLSCDouglas-fir Concora strength at 200 ml CSF is close to that of the GLSC hardwood pulp at 400 ml CSF level.

Ch 00 69 SUMMARY

Douglas-fir chips from Oregon were pulped with kraft green liquor to produce semi-chemical pulps for corrugating medium.The pulps had an average yield of 71% and strength properties marginally suitable for the manufacture of corrugating medium.Five cooking variables, chemical charge, bark content, chip size, sulfidity, and temperature, were investigated to study their effects on pulp qualities. Chemical charge is the most important cooking variable, and as the chemical charge decreased, the pulp yield rose, the tensile strength and bursting strength decreased, and the Concora strength improved.The temperature does not significantly affect the pulp yield, but as the temperature decreased, tensile strength decreased and the Concora strength improved.The variation of sulfidity also does not significantly affect the pulp yield, but it has some effect on the pulp strength.As the sulfidity increased, the stiffness, the tearing, the bursting, the tensile and the Concora strengths improved. As the bark content decreased, the pulp yield rose, the Concora strength, the tensile strength, and stiffness (MOE) improved, but the tearing strength decreased.As the chip size decreased, the tensile and Concora strengths improved. For reproducible results of the hypo no. test, a constant amount of well defiberated, never-dried pulp should be used.Further research on this subject seems necessary to find out the relationship 70 between the hypo number and lignin content of GLSC Douglas-fir pulp. A comparison of Taber stiffness and Concora strength shows a high correlation between them, and it appears that the Taber stiffness test could be used commercially to supplant the time-consuming Concora flat crush strength test. The effects of disintegrating in the Bauer refiner and refining in the PFI mill on the GLSC Douglas-fir hands heet properties are very important.The work dist-.ibution between the Bauer refiner and the PFI mill to lower the pulp freeness from 700 ml CSF to 200 ml CSF seems to be an important problem and should be investigated further. The Con.cora and tensile strengths are two of the most important strengths of corrugating medium.The maximum tensile strength of GLSC Douglas-fir pulp resulted from cooking with high chemical charge, small chip size, and high sulfidity.Tensile strengths are negatively correlated to pulp yields, which is normal for semi- chemical pulps. The tensile strengths of GLSC Douglas-fir pulps are about the same as those of NSSC Douglas-fir pulp, and are significantly higher than those of NSSC oak, GLSC oak, and GLSC Georgia pine pulps. The Concora strengths of GLSC Douglas-fir corrugating medium are slightly lower than those of other semi-chemical pulps.This low strength might be caused by fiber length differences, by chemical 71 composition differences (a- cellulose, hemicellulose, lignin, pentosans, extractives,...etc. ), or by a combination of the two.Further research work on this question is recommended. The chemical charge and temperature levels obtained for maximum Concora and tensile strengths are opposed to each other, but high sulfidity and low bark content are preferred for the maxima of both Concora and tensile strengths.Three suggestions for using GLSC Douglas-fir pulp are: Since the GLSC Douglas-fir corrugating medium has higher tensile strength than other commercial corrugating medium, it might be possible to cook the Douglas-fir chips with medium chemical charge, at medium temperature, and at high sulfidity to increase the pulp yield and Concora strength but with the sacrifice of some tensile strength. Because the Concora strength of the GLSC Douglas fir pulp increases with increasing refining work, and because the tensile strength of this pulp has not reached a maximum at 200 ml CSF, it may be possible to cook the Douglas fir chips with high chemical charge, high temperature, and high sulfidity to give high tensile and high bursting strength pulp.The Concora strength of the pulp can be increased with more refining work down to 200 ml CSF to reach the desired level of Concora strength without hurting the tensile and bursting strengths. 72 In summary, GLSC Douglas-fir pulpsaxe equivalent or slightly lower to other commercial semi-chemicalpulps in Concora strength, but equal or slightly superior to them intensile and bursting strengths. The pulp has a distinctly darker color than theNSSC pulp, and may be less bulky.The deficiency in Concora strengthcan be overcome with increased refining, and the slightly higher pulp yieldand elimination of the causticizing step make the GLSCprocess more attractive for corrugating medium. 7 3

CONCLUSIONS

In GLSC pulping, the cooking temperature does not strongly affect the pulp yield, which is in agreement with the conclusions

of Battan et al.(1975). Total alkali is the most important single variable affecting the pulp yield, and the two variables are negatively correlated. The sulfidity of the green liquor, which is normally important in the kraft mill operation, does not significantly affect the pulp yield, and this is in agreement with the work of Battan et al.

4,The pH value of the waste liquor can be used as an indication of the adequacy and the degree of utilization of the total chemical charge, but it cannot be used as an indication of the pulp yield or quality. For reproducible results of the Hypo number test, a constant amount of well defiberated, never-dried pulp should be used. The Concora strength is significantly affected by the total alkali (-), sulfidity (+), and bark content (-). The Concora strengths of GLSC Douglas-fir corrugating medium at 400 ml CSF level are lower than those of NSSC hardwood pulps (western oak, midwestern oak), NSSC Douglas-fir pulps, and GLSC hardwood pulps at equivalent freeness levels. The Concora strength increases with increasing refining work, 74 and the Concora strength of GLSC Douglas-fir corrugating medium at the 200 ml CSF level is very close to that of the GLSC hardwood corrugating medium (midwestern oak) at 400 ml CSF level. GLSC Douglas-fir pulps need more refining in order to develop Concora strengths comparable to other commercial semi- chemical pulps.This means higher refining costs and lower pulp freenesses, which may result in slower paper machine speed. The tensile strengths of GLSC Douglas fir pulps are about the same as those of NSSC Douglas-fir pulp, and are significantly higher than those of NSSC oak, GLSC oak, and GLSC Georgia pine pulps. The tensile strength is significantly affected by the total alkali

(+),chip size (-), and sulfidity (+).Tensile strengths normally are negatively correlated to pulp yields, but there the tensile strengths cannot be predicted by pulp yield alone, with any strong statistical significance. Tensile strength slowly decreases with increasing pulp yield up to 72% yield, and then rapidly decreases as the yield increases. Smaller chips produce pulps with higher tensile and Concora strengths. 75 The variation of bark content does not significantly affect the strength properties, but data suggests that lower bark content chips produce pulps with higher Concora and tensile strengths. The GLSC Douglas-fir corrugating medium has about the same burst strength as GLSC hardwood medium, but GLSC Georgia pine medium has higher tensile and bursting strengths. The Taber stiffness test is significantly correlated to the Concora strength of these pulps, and it appears that it could be used commercially to supplant the Concora test. The GLSC Douglas-fir pulp has a distinctively darker color than

the NSSC pulp, and they may be less bulky (i. e,greater denstiy) than the NSSC pulp.This is in agreement with Dawson (1974),

Charbonnier et al.(1974),and Battan et al. ' s work. In summary GLSC Douglas-fir pulps are equivalent or slightly lower than other commercial semi-chemical pulps in Concora strength, but equal or slightly superior to them in tensile and bursting strengths. The deficiency in Concora strength can be overcome with increased refining, and the slightly higher pulp yield (average 71%) and elimination of the causticizing step make the GLSC process more attractive for corrugating medium. 76

BIBLIOGRAPHY

Battan, H. R.; Ahlquist, G. S.; and Snyder, E.J."Green Liquor Pulping of Southern Oak for Corrugating Medium." Preprint, TAPPI Alkaline Pulping Conference, (Williamsbrug, Va. ), 1975.pp. 17-31. Becker, E, D. and Galdwell, H. G."An Evaluation of NSSC and Kraft Pulping of Ecuadorian Hardwoods for Corrugating Med- ium. " TAPPI 57 (12):117-119. 1974.

Bublitz, W. J. and Hull, J.L."Semi-Chemical Pulping of Douglas- Fir and Oak for Corrugating Medium." Internal report, Forest Research Lab., Oregon State University.Aug. 26, 1974. "Semi-Chemical Pulping of Douglas-fir Chips with Kraft Green Liquor and Neutral Sulfite Pink Liquor." Internal report, Forest Research Lab., Oregon State University.Dec. 1973. Casey, J. P.Pulp and Paper. New York: Interscience Publishers; Inc.,1966. Cederquist, and Defibra.tor.Sernichemical Cooking Liquor use in Green Liquor.German patent 2, 226,777. DOS Feb. 8, 1973. 6 claims.11 p. Charbonnier, H. Y.; Ruston, J. D.; and Schwalbe, H. C."Semi- Chemical Pulping of Pine with Green Liquor." TAPPI 57 (12): 108-112.1974. Chidester, G. H. ; Keller, E. L. ; and Sanyer, N."Semichemical and Chemirncehanical Pulping." in Pulp and Paper Manufacture, Vol.I.Edited by Ronald G. McDonald. New York: McGraw- Hill Book Co. 1969. Clayton, D. W."The Chemistry of Alkaline Pulping. "in Pulp and Paper Manufacture, Vol.I.Edited by Ronald G. McDonald. New York: McGraw-Hill Book Co.1969. Cochran, W. F., and Cox, G. M.Experimental Design.2nd ed. New York: John Wiley and Sons, 1957.p. 371. 77 Darmstadt, W. J.; Wangerin, D. D.; and West, P. H."Combustion of Black Liquor." in Chemical Recovery in Alkaline Pulping Processes, pp. 59-79.Edited by R. P. Whitney.Easton, Pa. Mack Printing Company, 1968. Dawson, R. L."A Compariosn of Neutral Sulfite and Green Liquor Semichernical Pulps in Corrugating Medium." TAPPI 57(12): 113-116.1974. Wenzl, Hermann F. J.Kraft Pulping Theory and Practice.New York: Lockwood Publishing Co., Inc.,1967. Lyubavskaya, R. A. et al.USSR patent 300,558.Issued April 7, 1971. McGovern, J. N."Semichemical and Chemirnechanical Pulping." in Pulp and Paper Science and Technology, Vol.I, pp. 281-316. Edited by C. E. Libby. New York: McGraw-Hill Book Co. 1962. Pollitzer, Stephanie."Capacity Survey Sees Annual 1.4% Increase. Pulp and Paper, 46(12):62-64.1972. Robeck, Robert F."Setting New Records for the Corrugated Box Industry. " Paper Trade Journal 157(43):36-37.Oct.22, 1973. Rydholm, S. A.Pulping Processes.1st corrected printing.New York: John Wiley and Sons, Ltd. 1967.Chap. 8 and 9. Swartz, J. N. and MacDonald, R. C."Alkaline Pulping. " in Pulp and Paper Science and Technology, Vol.1, pp. 160-239. Edited by C. E. Libby. New York: McGraw-Hill Book Co. 1962. Szwarcsztajn, E., et al.Przeglad Papier, 24(1):1-5.(in Polish) 1968. Vardheirn, S.Pa.pper och Tra. 49(9):613-619.1967. Whitney, R. P., ed.Chemical Recovery in Alkaline Pulping Process. pp, 1-14.TAPPI Monograph Series No. 32.Easton, Pa.: Mack Printing Company.1968, 78 Worster, H. E."Present State of Semichemical Pulping--A Litera- ture Review. " Paper Trade Journal, Aug. 20, 1973, pp. 3l- 37.

Yerger, H. J.,Jr., "Use of Oxidized Green Liquor in Producing Corrugating Medium from Northern Hardwoods. " TAPPI 56(9): 74-75.1973. APPENDIX Appendix Table 1.Simple linear regression of pulp qualities. (Y)= A +B x(X) Sign of Significance Level Variable(Y) Variable (X) R2 F value level Total solids in waste liq. pH of waste liq. 0.30 12. 00 0. 005 Power consumption Initial freeness 0.62 45. 70 0. 001

Power consumption PFI revolutions 0.31 12. 35 0.005 Yield Burst factor 200 ml CSF 0.29 11. 67 0.005 PFI revolutions Concora 0.40 18.70 0. 005 Bulk Stiffness, MOE 0.31 12.60 0.005

Concora Freeness 0.23 8.40 0.01 Concora Initial CSF 0.28 11.02 0. 005 Bulk Stiffness, MOE 1,000 PFI revs. 0.55 33. 72 0.001 Tensile strength Bursting strength 0.39 17.98 0. 005 Power consumption Freeness, ml CSF 0.31 12. 30 0. 005 Initial freeness Freeness, ml CSF 0.43 20. 76 0. 001

Concora Freeness, ml CSF 0. 51 29. 00 0. 001 Concora 1.8 cc/gm Bulk Stiffness, MOE 0.27 10.43 0. 005 Concora PFI revolutions 0.56 35. 59 0.001 Tensile strength Bursting strength 0.41 19.22 0.001

666 PFI revolutions Concora Freeness, ml CSF 0.70 66. 89 0. 001

333 PFI revolutions Concora Initial freeness O. 56 35.02 0.001 Appendix Table 2.Multiple regression equations relating cooking variables to pulping results. Cooking variables T. S. in waste liquor, g pH value in waste liquor x 100 Pulping yield cro x 10 ( B( I) T Value B( I) T value B(I) T value X(1) 43&5 3.36 52.90 0.73 -33.81 -0.77 X(2) - 20.9 -0. 16 -0. 15 -0. 002 -85.61 -1. 95 X( 3) 5.88 0.04 -122.80 -1.37 -18.16 -0.33 X(4) -196.7 -1.51 - 20. 13 -0, 28 62.96 1.43 X(S) -254.8 -1.96 -122.30 -1.70 4.56 0.10 X(6) - 54.46 -3.81 - 14.03 -1.77 4. 11 0. 85

X(7) 3. 52 0. 25 3. 16 -0. 40 12. 61 2. 61 X(8) - 22.57 -0.74 22.26 1.32 7.96 0.78 X(9) 14.63 1.02 - 11.66 -1.47 - 5.50 -1.14 X(10) 25.49 1.78 3. 33 O. 39 4.99 1.03 X(11) 6.43 -0.37 3.71 -0.38 6.61 1.14 X(12) 4.99 0.28 10.75 1.11 0.16 0.02 X(13) 1. 69 -0. 10 11. 92 1. 23 - 9. 52 -1. 61 X( 14) 9. 32 0.43 6. 17 0. 64 -0, 15 -0. 06 X(15) 1.52 -0.09 6.25 -0.64 3.29 0.49 X(16) 4. 56 0.26 5. 17 0. 53 - O. 89 -0. 15 X(17) 6. 80 0. 39 5. 67 0. 58 - 7. 77 -1. 31 X(18) 21.74 1.01 0.88 0.09 3.66 0.55 X(19) 9. 99 0. 57 5. 38 0. 52 - 4. 71 -0. 80 X.420) 20.05 O. 11 12. 80 1. 32 - 4. 14 -0. 67 Constant 810) 875.0 1105.9 838.1 Oo Note: Y = 8(0) + 1) x B(1) + X(2) x 2) +... +X( 20)x 8(20). Appendix Table 3.Multiple regression equations relating cooking variables to pulp properties ( 200 n1 CSF level)

Cooking Concora strength Breaking length Burst factor Tear factor variables T value B(I) T value B( I) T value P(I) T value

X(1) -21. 28 -4. 31 1, 229.80 O. 81 19. 60 4 26 22. 52 0.56 X(2) -23.03 -4.66 766.27 0.50 2.68 0.58 - 0.13 -0,003 X(3) - 0.92 -0. 15 2, 510.70 I. 32 5. 12 0.89 74.72 1.48 X(4) -19.01 -3.85 -625.93 -0.41 5.68 1.23 -20.18 -0.50 X(5) -14. 53 -2. 94 740. 24 0. 48 7. 69 1. 67 - 6. 20 -0. 15 X(6) 1.33 2.45 223.46 1.33 - 0.94 -1.86 - 4.53 -1.02 X(7) 0.83 1.53 175.63 -1.05 1. 19 -2. 36 - 1.66 -0. 37 X(8) - 2.84 2.46 165.39 0.46 - 1.45 -1.35 - 6.76 -0,71 X(9) 3.20 5.91 -177.19 -1.06 0.44 -0.88 3.59 0.81 X(10) 0.96 1. 76 267. 15 1. 59 -O. 06 -0. 13 0.71 0. 16 X(11) 2.21 3.32 193.92 0.94 - 0.04 -0.08 3.01 0.64 X(12) 1. 72 2. 59 830. 76 -4. 04 0. 30 -0.49 - 3. 12 -0. 57 X(13) - O. 17 -0. 26 479. 32 2. 33 0. 67 -1.08 - O. 12 -0.02 X(14) 1.33 2.00 503.99 -2.45 2.05 -3.30 2.38 0.44 X(15) 1. 35 2.02 293.68 1.43 - O. 19 -0. 32 - 1.87 -0. 34 X(16) 0.71 1.06 289.90 1.41 0.82 1.34 1.38 0.25 X(17) 1. 71 2. 56 663. 23 -3. 22 0. 20 0. 33 1.88 0. 35 X(18) 0.22 0. 33 -708. 27 -3. 44 0. 32 0. 52 4. 50 -0. 82 X(19) 0.72 1.09 33.05 0.16 0.05 -0.09 - 7.99 -1.46 X(20) - 0.92 -1. 38 393.40 1. 91 0. 17 -0.28 4. 26 0.78

Constant B(0) 166. 65 -2, 560.7 -43. 58 1.42 Note: Y = B(0) + X(1) B(1) + X( 2) x B(2) + + X(20) x B(20). Appendix Table. 3.(Continued).

Cooking MOE PFI revolutions Bulk x 100 variables B(i) T value B( I) T value 8( I) T value

X(1) 324.00 0. 32 -132.39 -0,22 -15,21 -0.28 X( 2) -241. 37 -0.24 -640. 62 -1. 06 40. 94 0. 75 X(3) -954.06 -0.77 493.57 0,09 33.27 0.49 X(4) 1, 754. 60 1.75 -1, 242. 80 -2.10 -44.17 -0.81 X(5) 496.01 0.50 397,96 -0.66 - 9.10 -0.17 X(6) 48. 34 0.44 32.35 0.49 - 5.27 -0.88 X(7) 93. 31 0.85 62.45 0. 94 - 3. 89 -0. 65 X(8) 114.63 0.49 151.23 -1.07 2.35 0.18 X(9) 65.03 -0.59 162.44 2.44 3.60 0,60 X(10) 63.19 0.57 47.54 0.71 - 5,14 -0.86 X(11) - 79.02 -0.59 39.-67 0,49 0. 63 0.09 X(12) 190.44 1.42 17.57 0.21 - 0.85 -0.12 X(13) 29.78 -0.22 35.76 -0.44 3.62 0.49 X(14) 180.84 -1.34 39.46 -0.48 10.38 1.41 X(15) 31. 32 -0.23 14.43 -0. 18 -6. 60 -0. 90 N 16) 168. 55 -1.25 33.99 0.42 -1. 63 -0.22 X(17) 91.12 0.68 32.53 0.40 1.63 0.22 X(18) 31.13 0.23 40.68 0.49 - 2.35 -0.32 X(19) 38.10 0.28 - 1.56 -0.02 - 5.35 -0.73 X(20) -211.58 -1.57 5.13 0.70

Constant 8(0) -1,043.30 4, 100.70 242.40 Appendix Table 4.Multiple regression equations relating cooking variables to pulp properties. (1, 000 PFI revolutions level)

Cooking Concora strength Breaking length Burst factor Tear factor variables 8(1) T value B(1) T value 8(1) T value IX 1) T value

X(1) -14.61 -1.45 1, 491. 20 0.53 16.80 3.00 14.59 0.47 X(2) - 6.20 -0.62 1,988. SO 0.70 7.22 1.29 -31.57 -1.01 X(3) -10.92 -0.87 3, 191. 10 0.90 6.86 0.99 59.40 1. 54 X(4) 13.47 1.34 612.27 0.22 9.30 1.66 -71.25 -2.29 X(8) - 3.03 -0.30 1, 735. 20 0.61 11.81 2.11 -33.46 -1.08 X(6) 0. 57 0.51 144. 93 0.47 - O. 98 -1. 60 - 3.05 -0. 89 X(7) - 0.43 -0. 39 -252. 82 -0. 81 1. 48 -2. 41 0. 08 2. 25 X(8) 0.39 0.16 155.40 0.23 1.20 - 0. 92 6.78 -0.93 X(9) - 0.56 -0.50 -322.68 -1.03 0.86 -1.39 8.19 2.40 X(10) 0.41 -0.39 160. 29 0.51 - 0.48 -0.78 3.32 0.97 X(11) 0.98 0.73 671.04 0. 18 - 0. 17 -0. 22 5. 14 1. 23 X(12) 1. 49 1. 10 -876. 99 -2. 29 - 0. 55 -0. 73 - 3. 09 -0. 74 X(13) 0.02 -0.01 603.27 1.58 0.08 0.10 0.99 -0.24 X(14) 1.8 1.37 -396.14 -1.03 1.42 -1.88 1.02 0.24 X(15) 1. 24 0.91 292. 80 0.76 0.57 0. 76 0. 59 -0. 14 X(16) 0. 52 -0. 38 226. 03 0. 59 0.21 0. 27 3.76 0. 90 X(17) 1. 11 0.82 -723. 16 -1.89 0.29 -0. 39 3. 27 0. 78 X(18) 0.76 -0.56 -832.23 -2.17 - 0.18 -0.23 1.22 -0.29 X(19) 0. 87 0. 64 - 46. 45 -0. 12 - 0. 68 -0. 90 7. 22 -1. 72 X(20) 1. 89 -1.40 322. 27 0. 84 - 0.29 -0. 39 7. 64 1. 82 Constant B(0) 76.04 -8, 679. 60 -59.64 188.78 Appendix Table 4.(Continued)

Cooking MOE x 0,1 Freeness, ml CSF Bulk x 100 variables 8(I) T value 8(I) T value 8(1) T value

X(1) 470.47 0.45 - 36.98 -0.26 20.86 0,43 X(2) 287.43 0.28 235.91 -1.67 4.97 0,10 X( 3) -610.98 -0.47 107.52 0.61 18.61 0.31 X(4) 1,479.00 1.43 268.39 -1.90 - 69.63 - 1.42 X(5) 838.31 0.81 137.29 -0.97 - 42.80 - 0.87 X(6) 0.92 0.01 2.99 0.19 2.80 0.52 X(7) 32,78 0.29 19.11 1.23 -0.67 - 0.13 X(8) 39.75 0.16 - 34.95 -1.06 3.50 0.31 X(9) - 31.62 -0.28 24.10 1.55 5.67 1.06 X(10) 6.33 0.06 13.61 0.88 -1.42 0.26 X(11) -106.97 -0.77 23.02 1.21 1.35 0.20 X(12) 172.74 1.24 4.13 0.22 0.37 0.06 X(13) 24.14 0.17 7.99 -0.42 1.36 0.20 X(14) -143.53 -1.03 12.11 -0.64 8.73 1.33 X(15) 5.60 0.04 2.00 -0.11 -6.87 1.04 X(16) 199.76 -1.43 12.39 0.65 1. 35 0,20 X(17) 69.31 0.50 9.01 0.47 3.73 0.57 X(18) 12.67 0.09 18.50 0.97 0.37 -0.06 X(19) 13. 78 0. 10 - 6.87 -0. 36 3. 99 - 0. 60 X(20) 212.04 -1.52 22.76 1.20 7.22 1.09

Constant 8( 0 ) -2, 231. 70 1, 100. 10 398. 66 Appendix Table 5.Multiple regression equations relating cooking variables to pulp properties. (1. 8 cc/gm Bulk level)

Cooking Concora strength Breaking length Burst factor Tear, factor variables 8(1) T value B( I) T value 8(I) T value 8(I) T value

15.39 2.93 - 38.65 -0.56 X(1) 4.52 0.61 1,511. 30 0.47 X(2) - 9.90 1.35 382.01 0.12 4,47 0.85 - 75.55 -1.10 10. 38 1. 59 12. 82 0. 15 X(3) 22. 45 2. 45 5, 342. 40 1. 34 X(4) -16.37 2.22 -2,023.90 -0.63 1.19 -0.23 -112.34 -1.64 0. 63 X(5) -1. 99 0. 27 2, 005. 00 0.63 1.64 2. 22 43.37 X(6) 1.06 2.30 105.24 0.30 - 1.36 -2.36 1.83 -0, 24 -3.01 4,04 0,54 X(7) - 0.81 1.00 -115.51 -0.33 1.74 -1. 90 4, 97 0. 31 X(8) -3. 62 0.21 - 2. 75 -0.004 - 2. 32 X(9) 3.20 3.95 - 72.41 -0.21 0.01 0.02 8,53 1.13 X(10) - 1.30 1.61 52.25 -0.15 - 0.86 -1.50 4.29 0,57 X(11) 0.61 0.62 33.17 0.08 - 0.05 -0.07 10.87 1.18 X(12) - 2.13 2.15 -1, 233. 70 -2.86 1.05 -1.49 0.55 0.06 X(13) 0.23 0.24 780.61 1.81 0.95 1.35 1.37 0.15 0.49 X(14) 1.49 1.50 -208.99 -0.49 0.67 -0.96 4,50 -0.73 X(15) 1.11 1.12 331.86 0.77 1.20 1.69 6.70 X(16) 0.48 0.49 423.28 0.98 O. 95 1. 35 9.12 0.99 X(17) 2. 99 3. 01 -591 66 -1. 38 O. 08 0. 11 4,00 0.43 X(18) -1. 76 1. 77 -1,016 60 -2. 36 - O. 30 -0. 43 5, 05 0.55 X(19) - 0.50 0.51 -168.26 -0.39 0.68 -0.96 10.,58 -1.15 X(20) - 1.14 1.15 416.75 0.97 -0.42 -0. 60 8.00 0.87

Constant 8(0) 74.49 - 3,797. 10 - 35. 29 454.47 Appendix Table 5.(Continued))

Cooking MOE 100 x log revolutions Freeness, ml, CSF variables B( I) T value B(I) T value 8(1) T value

X(1) 746. 03 1. 37 - 40.86 0.49 227.89 -1.23 X(2) 48.56 0.89 - 27.36 0.33 -219.81 -1.18 X(3) 278.73 0.41 247.83 2.40 -219.26 -0.95 X(4) 533.03 0.98 - 305. 51 - 3.68 99. 10 0.53 X(5) 935.02 1.72 39.60 -0.48 173.80 -0.94 X(6) - 75.46 -1.26 7.73 -0.85 12.25 0.56 X(7) - 20.96 -0.35 1.73 - 0.19 33.24 1.63 X(8) -134.87 -1.06 35.61 - 1.84 5.57 -0.13 X( 9) 98.76 1.65 33.11 3.63 11.23 -0.55 X(10) - 41.27 -0.69 -6.73 -0.74 34.97 1.71 X(11) - 24. 36 -0. 33 1.81 0.16 31.51 1.26 X(12) 92.05 1.26 - 21.62 1.93 61.51 2.46 X(13) 4.55 0.06 19.67 1.76 13.85 -0.55 X(14) 100.40 -1.37 17.69 1.58 8.75 -0. 35 X( 15) 7.52 1.03 7.75 0.69 21.37 -0.85 X(16) -124. 83 -1. 71 6.05 0.54 6.02 0.24 X(17) 72.46 1.00 14.32 1.28 19.63 -0.78 X(18) 77.17 -1.05 2.77 0.26 24.01 0.96 X(19) 49.61 0.68 11.11 0.99 28.62 1.14 X(20) -206.59 -2.82 1.18 0.11 5.24 -0.21

Constant B ( 0) -1, 166.10 839. 90 1, 054. SO Appendix Table 6.Multiple regression equations relating cooking variables to pulp properties. (0 PFI revolutions level)

Cooking Concora strength Breaking length Burst factor x 100 Tear factor variables B(I) T value 8( I) T value 8( I) T value B( I) T value

X(1) 10. 21 0. 64 1, 173. 40 0.93 718.48 1. 86 64. 28 1. 85 X(2) 10.62 0.67 2, 06S. 70 1.64 467.59 L21 51.83 1.33 X(3) 4. 62 0. 23 1, 523.40 0.97 291. 74 0. 61 34. 94 0, 76 X(4) 9. 29 0.58 170. 06 0. 13 236.05 0. 61 6. 60 0. 17 X(5) 7.03 0.44 1, 040. 40 0.82 472.21 1. 20 36.68 0.90 X(6) -1. 19 - 0. 68 0.41. -0.03 - 45. 25 -1.07 -4. 27 -0.99 X(7) - 1.69 - 0.96 241.13 -1.74 78.74 -1.85 - 10.89 -2.55 X(8) - 0.33 - 0.09 - 62.70 -0.21 70.60 -0.78 - 11.56 -1.27 X(9) - 1. 19 - 0. 68 106.46 -0.77 31.74 -0. 75 -3. 52 -0. 82 X(10) - 0.94 - 0.54 1.04 -0.01 - 30.72 -0.72 3.64 -0.85 X(11) - 0.55 - 0.22 79.55 -0.47 - 33.19 -0.64 1.43 -0.27 X(12) - O. 93 - 0.43 417. 59 -2.46 - 72. 16 -1. 38 6. 33 -1. 21 X(13) 0.20 0.09 272.71 1.61 17.56 0.34 3.82 0.73 X(14) 0. 20 0.09 151.60 -0.89 53.48 -1. 03 -S. 93 -1. 13 X(15) 0. 82 0. 38 172. 80 1.02 67. 22 1. 29 8. 92 1. 70 X(16) 0.05 - 0. 02 1. 39 -0.01 7.06 -0. 14 1. 43 -0. 27 X(17) - 0. 30 - 0, 14 285. 64 -1.68 21.09 -0. 41 -0.93 -0. 18 X(18) - 0.93 - 0.43 247.39 -1.46 6.22 0.12 0.42 0.08 X(19) - 0.18 - 0.08 4.40 -0.03 13.55 -0.26 -0.58 -0.11 X(20) - 0.05 - 0.03 114. 33 0. 67 _ 8. 34 -0. 16 4. 57 0. 88

Constant B(0) -46. 99 -6, 858. 6 -2, 459. 00 -159.54 Appendix Table 6.(Continued)

Cooking MOE x 0. 1 Freeness, ml CSF Bulk x 100 variables E(I) T value 3(1) T value 8(I) T value

X(1) 8, 244. 70 1.74 73.43-0.46 119.57 -1.26 X( 2) 2, 370.20 0.50 103.90 -0.65 - 14.98 -0. 16 X( 3) 3, 952. 20 0.67 51.08 0.26 - 88.02 -0.75 X(4) 4,088. 40 0.86 68.06-0.42 - 82. 39 -0.87 X(5) 4,942. 50 1.04 38. 11 -0.24 -142. 76 -1.50 X(6) 669. 13 -1. 28 11.45 0. 65 3. 07 0. 29 X( 7) 340.52 -0. 65 14. 19 0.81 5.57 0. 54 X(8) 1, 345. 00 -1.24 5.41 0.15 31.23 1.41 X(8) 212.61 -0.41 8.44 0.48 2.19 0.21 X(10) 254. 03 -O. 49 8.69 0.49 3. 81 0. 34 X(11) - 318.10 -0.49 7.65 0.35 -0.92 -0.07 X(12) 286.93 -0.45 1.14 -0.05 14. OS 1. 10 X( 13) 132.65 0.02 0.15 0.01 -1.54 -0.12 X(14) 731.97 -1.15 6.11 -0.28 24.22 1.90 X(15) 850.85 1.33 0.13 -0.61 - 23.08 -1.81 X(16) 316.54 -0.50 3.77 0.08 6.83 0.54 X(17) 92. 95 -O. 15 5.27 0. 24 6. 09 0.48 X(18) 283.87 -0.44 2.24 0.10 0.55 0.04 X(19) 141.59 0.22 8.77 -0.41 -4.44 -0.35 X(20) 433. 381 -O. 68 0.23-0.01 14.96 1. 12

Constant 13(0) -26, 092.00 1, 039.40 924. 47 89

Appendix Table 7.Original data. 90 COOK FGL1. A3B1C253T3 YIELD= 79.85

ORIGINAL DATA INTERVALS 12,3, 4 BEAT I NO 7.0n :Dania CSF 719 635 4/4 233 CONCORA 9. 1 26.9 49.7 BULK 3.2 2.4 2. 1 2.0 BREAKING LENGTH 1288 3974 4311 BURST 'FACTOR 14.9 96).6 TEAR FACTOR 111. 4 122.5 94. 7 77.7 STIFF. (MOE 75875 20'580 224381 CONSTANT FREENESS,600, 400, 200 ML CSF BEATING 677 11.364 CONCORA 98.c) 45 51.5 BULK 2. 4 2.1 2. BREAKING LENGTH -z.15A 4000 4372 BURST FACTOR 15. 7 20.4 23.0 TEAR FACTOR 118. 1 93. 3 74.? STIFF. 011-3E::1 210241 227439 271130 CONSTANT BEAT I NG, 333,667,1000 PF I REVS CSF 614 405 97C-1' coNcoRA 28. 1 40. 2 49.? BULK: 2.4 2.1 BREAK I NO LENGTH 3,388 7e.c49;71 4311 BURST FACTOR 15. 4 20, 3 TEAR FACTOR 19. 9 ci 77. 7 STIFF. (NOE ) 2n91P.0 226264 L I N.REGR. -BULK,1. 6,1.8,2. 2. 2CC/GM LOG BEATING 4. 2 3. 7 2.? =-Z 559 X + 8. 31.4 R-SQ. =8.977 F= 86.883 CSF 209 278 348 417 = 347. 928 X +-348. 178 R-SQ. = O. 732 F= 5. 451. CONCORA 57.6 51.4 45.1 38.8 =-31.332 X + 107.754 R-SQ. =0. 933 F= 27. 806 BREAKING LENGTH 5231 4733 4235 3736 =-2492. 103 X + 9218. 862 R-SO. =O. 986 F= 136. 448 BURST FACTOR 27. 4 24.? 21. 9 19. 1 =-13. 912 X+49. 707 0. 983 F=115. 760 TEAR FACTOR 87.3 87.6 92.0 qtc.4 V= a 834 X + 48. 343 R-SQ. = 0. 362 F=1..137 STIFF. (. MOE 3.1844E; 288510 258575 998639 =-149677. 443 X + 557929. 467 R-S.= 0.983 F= 118.331 X - MEAN 439 COOKFGL3A A3B3C253T3 YIELD= 72. 250

ORIGINAL DATA,INTERVALS 1, 2,3,4 BEAT I NO 0 300 1000 CSF 745 647 423 228 CnNCORA 8. 4 22. 4 32.5 42.8 BULK 4. 0 2. 9 2.7 BREAKING LENGTH 1005 2454 7:1686 5027 BURST FACTOR 4. 4 15. 4 21. 7 24. 9 TEAR FACTOR 11E1. 1 176. 4 148.? 128. 8 STIFF. (MOE 37112 125657 149868 165400 CONSTANT FREENESS,600, 400,200 ML BEATING 373 691 1050 CONCORA 25. -7q. 0 43. 4

BULK 9 . BREAK I NO LENGTH 2712 3844 5'7,19 BURST FACTOR 16.? 22. 1 25. 4

TEAR FACTOR 17afz. 146. 3 126. 1.71 STIFF. I:. MOE 13077:7 151700 167630 CONSTANT BEAT I NO,333, 667,1.000 PF REVS CSF 414 CONCORFi s.7:. 9 4. BULK 2. q 2. 6 2.5 BREAK I NG LENGTH 2571 3750 5027 BURST FACTOR 16. 21. 9 24: 9 TEAR FACTOR 173. :3 147. 7 .128. 8 STIFF. (MOE) 127C1F;7:: 150608 if.:;5400

UN. REGR. -BULK, 1. 6, 1. 8, 2. 0,2. 2CC/GM LOG BEATING 5. 1 4. 7 4.7: 3. 145 X + 8.547 R-91 = 0. 985 F= 133.197 CCFEU 141 'N-19 262 = 303.294 X +-404. 866 R-91 = 0.718 F= 5.083 CONCORA F.P1. 51. 6 47.IA =-23.169X + 97.966 R-SQ. = 0. 903 F= 18. 630 BREAKING LENGTH 6520 6030 5540 5049 =-2450. 154 X + 10439. 824 R-91 = 0. 853 F= ii 572 BURST FACTOR 36. 1 33. 4 6 T.?.9 =-13. 740 X + 58.100

R-SQ. = 0. 969 F= 62. 349 TEAR FACTOR 172.8 168. 3 163. :3 159. 4 410 X + 208. 661 R-SQ.= 0.262 F= 0.709 STIFF. (mOE) 245109 227405 s.0970S 191998 =-88518. 922 X + 386739. 492 R-SO. = 0.999 F=2623. 837 X - MEAN =3. 019 COOK FGL4 A3B3C253T1YIELD= 72. 620

CONSTANT FREENESS, 600, 400, 200 ML CSF BEAT I NG 445 Ric:.5 1175 CONCORA ...;:q. 5...1 *7:3. 5 48. 7 BULK 2. 4 2. 2 2. 0 BREFIK I NG LENGTH 3136 4026 4913 BURST FACTOR 16.7 92. 1 27. 1 'TEAR FACTOR 118. 8 101. 2 RR, i.--; STIFF. ( MOE ) 158191 191408 197578 CONSTANT BEATING 333, 667, 1000 PF I REVS CF 677f. 595 313 CONCORFI 94. 9 3-2f: 425 BULK 24 2: 21 BREAK I l',11.3 LENGTH 2987 3457 4412 BURST FACTOR 15. 6 19. 0 24. 3 TEAR FFICTOR 123. 5 109. 2 95. 7 ST I FF.

L I t-4. REGR. -BULK,1. 6,1. 8,2_ 0,2. 2 CC/GPI LOG BEAT I r4G 4. 7 4.1 3.5 3.0 =-2.817 X 4- 9.157 R-50. = 8.915 F= 21.550 CSF 161 240 319 Y = 394.872 X+-478.685 R-SQ.= 8.745 F= 848 CONCORA 53.7 47.5 41.2 35.0 =-31.252 X + 103.728 R-SQ. = 835 F= 10.129 BREAKING LENGTH 5915 5297 4678 4060 Y =-3091. 5131 X + 10861.391 R-S 0.996 F= 465.667 BURST FACTOR 6 20. 5 -15.777 X + 55.195 R-50. = 0.982 F= 111.41 TEAR FACTOR 134. 7 135. 0 135. 3 17:5. = 1.487 X + 132.305 R-SQ. = 0.000 F= 0.001 STIFF. ( MOE ) 275200 24655c:; 217911 1549267 =-143222. 624 X + 504356.468 R-SQ. = 0.990 F= 206.197 X - MEAN = 515 94 COOK FGL6 F14B2C354T2 YIELD= 71. 920 ORIGINALDATA It-4TERVALS 1, 2, 3, 4 BEATING 1-47,Fda 1000 CSF 77:7: 642 438 199

CONCORA . 24.0 48. 51. 2 BULK 3.A 2.3 2.1 2.0 BREAKING LENGTH 1582 -;-17-120 3715 5056 BURST FACTOR 7. c 20.3 25. 4 A TEAR FACTOR 121. 8 139. R j_cif-7.. R7. 7 STIFF.(MOE) 78R-z.R 224152 384710 CONSTANT FREENESS,60a. 400, 200 ML CSF BEAT I NO 372 706 999 CONCORA 27. 42.5 51.1 BULK 2.3 2.1 2.0 BREAKING LENGTH 3163 3928 5050 BURST FACTOR 21.3 6 9 TEAR FACTOR 103.1 87. 8 STIFF.(MOE) 173256 249680 CONSTANTBEATING,333, 667, 1000 PFI REVS CSF 427 199 CONCORA 41.4 51.2 BULK 2.1 2.0

BREAKING LENGTH : 3779 5056 -BURST FACTOR 20. 7 25.8 33.0 TEAR FACTOR 136. lc; 105.1 87.7 STIFF. (MOE) 231797 384710

LIN.REGR. 6 1. 8, 2. 0, 2. 2cr/Gri LOG BEATING 4. 4 8 3.1 2.5 Y=-3.124 X + 9.389 R-SQ. = 0. 962 F= 50. 047 CSF 155 249 343 = 468. 477 X +-594. 370 R-SQ.=a752 F= 6.050 CONCORFi 61. 1 53..1 45. 1 37. 1 Y =-39. 991 X + 125. 072 R-SQ.=a911 F= 29.555 BREAKING LENGTH 5680 5050 4421 3791 =-31.46. 943 X + 10714. 707 R-SQ.= 0.912 F= 28.851 BURST FACTOR 5 29 7 25. 0 =-23. 771. X + 77.282 R-92. = 0. 967 F=57. 962 R TEAR FACTOR Cr?. 913.5 104. 1 109. = 28. 285 X + 47. 576 R-SQ. = 0. 312 F= 0. 906 STIFF. (MOE) 404627 7:0AR12 248904 Y =-259539. 179 X + 819890. 088 R-SQ. = 0.773 F= 6.801 X - MEAN = 342 COOK FG-L7 A2B4C152T2Y I ELD= 71. 890 ORIGINAL D,ATA, INTERVALS 1, 2, 3, 4 BEATING 650 10:710 CSF 705 659 433 176 CONCORA 15.3 24.? 45. 0 BULK: 4.3 2.8 2.7 2.5 BREAK I NO LENGTH 729 163E: 2267 2535 BURST FACTOR 2. 3 7.8 7.7 8. 1 TEAR FACTOR 69. 5 -.1.09. 9 89. R La 5

ST I FF.(. moE) 31143 Rci;=,87 . 14/CF.65 CONSTANTFREENESS.. 600, 400, 200 ML CSF BEAT I NG 391 695 957 CO NC ORA 17. 8 27. 3 43. 1 BULK 2.8 2.7 BREAK I NO LENGTH 181712 2301 2510 BURST FACTOR 7.8 7.8 8.1 TEAR FACTOR 104. 1 R7. la 7171. STIFF. (MOE) 86582 108828 142522 CONSTAt-T BEAT I NG..333, 667, 1.000 PF I REV CSF 637 421 176 CONCORF: 16. 2 25. 7 45. 0 BULK 2. 8 2.7 2.5 BREAK I NO LENGTH 2535 BURST FACTOR 7. :3 7.7 8.1 TEAR FACTOR 107. 4 88.8 68.5 ST I FF. ( moE 82872 1053.7-:1 LIN.REGR._ -BULK,1.6..1. 8,2. 0..2. 2 CC/Gti LOG BEATING 4. 7 4. 3 4. n 3. 6 =1 755 X + 7. 469 P-SQ.= 0. 999 F.:: 3455. 359 CSF 1891 223 265 307 fr' = 212. 242 X +-159. 465 R-S.= a 4861.889 CONCORFi 46. 7 43. 5 40. 2 36. 9 =-i6.308 X + 72.818 = O. 601 Fr- 3. 007 BREAKING LENGTH 3191 317102 9819 =948. 560 X + 4709. 083 R-SO. = a 7 15. 742 BURST FACTOR 11. 6 10. 9 10. 2 9. 9 =3. 4% X + 17.223 R-91 = O. 988 F= 170. 193 TEAR FACTOR 97 7 95. 9 94. 0 I? =9. 126 X + 112. 251 R-SQ. = O. 141 F= O. 323 STIFF. (MOE) 170213 148578 137761 Y =54087. 619 X + 256753. 264 = 0.884 F= 8.220 X - MEAN = 3. 075 96 COOKFGL8 A282C3S2T2 YIELD= 75. 120

ORIGINAL DATA INTERVALS 1,2, 3, 4

BEAT I NO . 7..ng 650 1171A0 CSF 762 642: 513 242 CONCORA S. 6 29.1 45.9 BULK 4. 3. 1 2.8 2.6 BREAKING LENGTH 116'; 2993 3805 4R99 BURST FACTOR 3;5 7. 9 10.7 12. 7 TEAR FACTOR :31. 9 2 127.1 .i05.5 STIFF. (MOE ) 94561 113570 137001 CONSTANT FREENESS,600, 40a.200 !ILCSF BEATING 416 796 1054 CONCORA .:1)5. 36. 1 48.5 BULK 2.7 BREAKING LENGTH 422:2 49:3R BURST FACTOR 8.8 1. 6 13. 0 TEAR FACTOR 120. 5 1 102. 2 STIFF. (MOE ) 100849 123340 14c:632 CONSTANTBEATING. 333,667,1000 PF IRE' 5 CSF 631 517671 242 CONCORA 24. 4 45. 9 C. BULK 3.1 2. 2.6 BREAKING LENGTH 3071 3854 4829 BURST FACTOR R.2 10. 8 12. 7 TEAR FACTOR 118. 12A. 0 105. Fi STIFF. (.10E) 114685 1-.Z7001

L I N. REGR. -BULK, 1. 6, 1. 8, 2.a.2. 2 CC/G11

LOG BEFiTING - 5. 5 5.1 4.6 4.2 V=-2.239 X + 9.084 R-SQ.= 0.965 F= 55.205 C:SF 56 119 182 245 = 316.225 X +-450. 366 R-SQ.= 0.756 F= 6.198 CONCORA 63. 0 58. 3 53.5 48. 8 + 100. 666 R-99. = 0.885 F= 15.434 BREAKING LENGTH 7008 6511 6013 5516 Y =-2486.443 X + 10986. 214 R-91 = 8.972 F= 68.562 BURST FACTOR 18. 6 17. 3 1F.;. 14. 7 =-6.424 X + 28.848 R-91 = 0. 967 F= 59. 058 TEAR FACTOR 144. 8 140. 0 130. 4 089X + 183. 366 R-SO.= a577 F=2.733 STIFF. c. MOE 212410 196776 181142 165508 =-78170. 347X + 337483. 016 R-SO. = 0.999 F= 1409. 221 X - MEAN = 3. 12:2 COOK FGL9 A383C253T3 YIELD= 71. 310 ORIGINALDATA, INTERVALS 1,2, 3, 4 BEATING 700 650 CSF 677 515 7::59 195 CONCOF:A 14. 3 31. 8 42. 5 45. 1 BULK 2.7 2. 2.2 BREAKING LENGTH 2204 4262 4711 549.1 BURST FACTOR q. 21, 1 25. 1 TEAR FACTOR 164. 9 123.PI 104. 7 91. 2 ST I FF. (MOE ) 100686 179741 185332 123:673 CONSTANTFREENESS,600, 400, 200 ML CSF BEATING .143 989 CONCORA 22. 6 -;:c), 7 45. 0 BULK 2.5 2.2 2.5 BREAKING LENGTH 3182 4593 5468 BURST FACTOR 15. 2 24.0 29.3 TEAR. FACTOR 145. 0 109. 5 91. 6 STIFF. (MOE) 138262 183863 125553 CONSTANT BEAT I NG, 667,1000 PF I REVS CSF 351 195 CONCORA 42. 6 45.1 BULK 2. 2 BREAKING LENGTH 4748 5491 BURST FACTOR 95. 29.5

TEAR FACTOR 104. 171 91. 2 STIFF. c. MOE 182396 122:673 L IN.REGR. -BULK,1. 6,1. 8, a et,2. 2 CC/GM LOG BEATING 5. 9 4. =-4.632 X + 13.269 R-SQ. = 0.664 F= 3.958 CrF 95 178 262 346 = 418.309 X +-574. 581 R-SQ. = 0.248 F= 0. 658 CONCORFi 67. 9 59. 4 51. 0 42. 6 Y =-42. 170 + 115. 352 R-SQ. = 0. 550 F=2. 447 BREAK I NO LENGTH 7372 6557 5782 5008 =-3873. 113 X + 13528. 579 R-SO. = 0. 461 F= 1. 711 BURST FACTOR 40. 2 35. 6 31. 0 26. 4 =-23.862 X + 77.104 R-SQ. = 0.452 F= 1.649 TEAR FACTOR 47. 2 65. 8 3 101. 4 = 90. 268X +-97. 234 R-SQ. =0. 480 F= 1. 848 STIFF. C. MOE 278654 246516 214377 182r23e4 Y =-168692. 016 X + 535761. 449 R-50. = 0. 897 F= 17. 400 X - MEAN = 2. 417 98 COOK FGL10 A4B2C1S2T2YIELD= 69. 690 ORIGINAL DATA,INTERVALS 1, 2, 3, 4 BEATING 300 /570 1000 CSF 568 235 CONI:ORA Da. 8 21. 2 .1cf.f 44. 4

BULK 2. 9 9.9 S' 2. 1 - BREAKING LENGTH 2280 4510 5707 7166 BURST 'FACTOR 8. 4 14.4 19. 2 97. 9 TEAR FACTOR 138. 143.4 142. 5 97.9 STIFF. (MOE ) 79-4,12 128743 168161 188566 CONSTANT FREENESS.,600, 400,200 MLCSF BEATING 221 561 1122 CONCORA 18. 4 32.8 41::.9 BULK 2. 9 2.7 1.9 BREAKING LENGTH 3931 5355 7703 BURST FACTOR 12. 8 17. 8 30. 1 TEAR FACTOR 142. 1 142. 8 81. 5 STIFF. (MOE) 115668 156567 19)=.084 CONSTANT BEAT I Na. 333, 667,1000 PF I REVS CSF 547 332 CONCORA - 22.7 37.6 44. 4 BULK 2.9 2.6 2.1 BREAK I NG LEN13TH 4518 5697 7166 BURST FACTOR ±4.9 19.2 27.2 TEAR FACTOR 143, 3 142. 5 97. 9 ST I FF. ( moE 132294 167806 1885F7.6

L I N.REGR. -BULK,1. 6,1. 8,2. 0,2. 2 CC/GM LOG BEATING 4. 1 3. 7 3.3 2.9 =-2. 048 X + 7.412 R-91 = 0.336F= t813 CSF 66 162 257 V = 477.815 X +-792.1 R-SQ. = 0.823 F= 9. 276 CONCORFi 63. 4 56. 9 49. 42.8 V =-34. 337 X + la.345 R-SQ. = 0.796 F= 7.826 BREAKING LENGTH 9409 7640 6755 Y =-4423.323 X + 1603. 555 R-SQ. = 0. 727 F= 5. 324 BURST FACTOR 36. 32. 4 =-1a43 X + 65.685 R-9/ = 8.858 F= 1133 TEAR FACTOR 81. 1 90. 9 1510. 110.4 = 48. 690 X + 3. 240 R-91 = a 785 F= 7. 302 STIFF. ( MOE ) 243705 183156 Y =-100914. 240 X + 405167. 396 R-Sa = 0. 696 F= 4. 582 '-MEAN = 2. 616 99 COOKFGL11 A383C253T5 YIELD 70. 500 ORIGINAL DATA I NTERVALS 12, 3, 4 BEATING 0 300 650 1000 CSF 666 469 360 165 CONCORA 15.4 32. 8 42.6 48. 9 BULK 3. 1 2.0 2.1 BREAKING LENGTH 2559 4787 5750 7866 BURST FACTOR 8. 1 99.8 26.8 28. 6 TEAR FACTOR 143. 9 141. 8 124. 6 127. 3 STIFF. (MOE) 81457 178263 259145 233878 CONSTANT FREENESS,600, 400,200 ML CSF BEATING 101 522 937 CONCORA 21.2 39.0 47. 8 BULK 2.8 2.1 2.1 BREAKING LENGTH 3305 5396 7486 BURST FACTOR 13.1 25. 4 28. 3 TEAR FACTOR 143.2 130. 9 126.8 STIFF.

L I N. REGR. -BULK, 1.. 6, 1. 8, Z. 0 2. 2 CC/GM LOG BEATING 4. 2 3.? 3.1 2.6 V=-2.753 X+8. 612 R-SQ.=O. 993 F= 28i076 CSF 141 212 282 353 =353. 361 X 4-424. 237 R-SQ.= 8.738 F= 5.487 CONCORR 56. 506 451 39? Y -27.285 X+99.53? R-SQ.= 8.889 F= 15.969 BREAKING LENGTH 8144 7395 6645 5896 =-3746.1i4 X+14137. 529

R-50..=8.741 F= 5.726 BURST FACTOR 35. 7 32. 28.4 24.8 =48.196 X+64.818 R-SQ.= 8.982 F= 186.649 TEAR FACTOR 123. 0 125. 9 128. 9 131. 8 = 14. 751 X + 99. 375 R-SQ. O. 577 F= 2. 725 STIFF. (MOE> 304150 274224 244299 214373 =-149627. 636 X + 543554.079

R-SQ.= 0. 924 Fr-. 24. 429 X - MEAN = 100 COOKFGL12 A2B4C321-4 YIELD= 72. 370 ORIGINAL DATA, INTERVALS 1, 2.. 3, 4 BEAT I NG 0 300 F.5n 1000 CF 716 610-.1...ef.S1 146

CONCORA 1171.7.: 2 9. R 3 7 42. F. BULK --Z. 0 25 22 2. 1 BREFtK I NG LENGTH 1-474; ssRs.f.:: 3422 3RF,R BURST 'FACTOR 5. 0 19. 5 15. 5 15. 7 TEAR FACTOR 105. 5 114. 7 90. 4 72: 7 STIFF. ( MOE ) 73861 151239 227291 231951 CONSTANT FREENESS, 600, 400,200 MI_ CSF BEATING 314 595 912 CONCORA 23. 4 -::::4. 5 41. i BULK 9.5 9. -:: 2. 2 BREAK: I NG LENGTH 2852 3329 3756 BURST FACTOR 12. 6 15. 1 15. 6 TEAR FACTOR 113. 7 94. 9 77. 2 STIFF. (MOE ) 154293 215379 230781 CONSTANT BEAT I NG, 333, 667, 1000 PFI REV-'S- CSF 5E 351 146 CONCOR A 24. 1 37.n 49. BULK .9. 5 2: 2. 1 BREAK I NG LENGTH 4..-0°....1 3.443 7:Rfv,R BURST FACTOR 12. 8 15. 5 15. 7 TEAR FACTOR 112. 4 89.r. 72.7 STIFF. (MOE) 158482 227513 231951

LIN.REGR. -BULK, 1. 6, 1_ 8, 2. 0, 2. 2 CC/GPI LOG BEATING 5.1 4.4 3.7 3.0 =-3.460 X + 10.595 R-SQ. = 0. 941 F= 31.614 CSF 8 70 187 304 = 586.276 X +-985. 592 R-SQ.= a806 F= 8. 331 CONCORA 59. -.I: 52. 0 44. 8 37. 6 =-36. 116 X + 117. 043 R-SQ. = 0. 955 F= 42. 842 BREAKING LENGTH 5262 4708 4153 35-99 =-2771. 650 X + 9696. 784 R-SL= 8993 F= 296. 731 BURST FACTOR 23. 1 20. 6 18. 0 15. 5 =-12. 645 X + 43. 331 R-S. = 0. 986 F= 138. 486 TEAR FACTOR 74. 7 81. 1 87. 4 = 31. 875 X + 17. 319 R-SQ.= 0.463 F= 1.722 STIFF. MOE) 2:2: 3 6 9 4 295397 25R701 220605 Y =488480. 453 X + 635262. 313 R-SQ. = 0. 980 F=%493493 - MEAN = 2. 463 101 COOKFGL13 Fi4B4C1S2T4 YIELD= 69. 150 ORIGINAL DATA INTERVALS 1, 2, 3, 4 BEATING la -z.nia 650 CSF 738 r.:Pic) -:'-59 219 CONCORA 7. 7 22. 0 37. .:-.. 43. 9 BULF::: :9 20 2E 2.5 BREAKING LENGTH 872 - *)734 3718 '7.921 BURST . FACTOR 4. 3 13. 5 20. 5 24. 0 TEAR FACTOR qc). 7:: 155. E.: 144. 6 120. 9 STIFF. (MOE ) 45867 117419 1455; 175447 CONSTANTFREENESS,600, 400, 200 ML CSF BEAT I NO 313 1048 CONCUR A 22. 5 34. 7 44. 8 BULK 2.4 BREAK I NO LENGTH 2769 3557 BURST FACTOR 13. 7 ic.t. 24.4 TEAR FACTOR 155. 4 146. 5 117. 7 STIFF. if. MOE ) 118433 140975 179498 CONSTANT BEAT It4G, 3.73, 657,1000 PFI REV-"S CSF 219 CONCORA 23. 4 e .:s 4:9 BULK 2.6 BREAK I MG LENGTH 779R 3921 BURST FACTOR 14. 2 20.6 24.0 TEAR FACTOR 154. 8 143. 5 .120. 9 STIFF. ( MOE ) 121-711n2 147017 175447

LIN. REGR. -BULK, 1. 6, 1. 8, 2.0,2. 2 CC/GM LOG BEATING 5. 0 4. 6 4.2 3.8 -a896 X + 8.371 R-SQ. = 0. 957 F= 44. 323 CCF 147 213 = 332.848 X +-519.069 R-SO. = 0.853 F= 11.631 r:ONCORA 61. 51.9 47.1 Y =-24.085 X+ 100.886 R-Sa. = 0. 944 F= 33. 975 BREAK I NO LENGTH 5806 4954 4528 =-2131. 026 X + 9215. 787 R-91 = 0. 997 F=727.497 BURST FACTOR 34.la 31. 4 28.7 26.1 Y =-13.116X + 54.969 R-91 = 0. 974 F= 75. 436 TEAR FACTOR 161. 4 157. 152. 5 148. 1 =-22.252 X+ 197.829 R-SO. = 8.332 F=0.993 STIFF. (MOE) 239593 223728 205863 -I88998 =84324. 842X + 374512. 440 R-91 = 0. 985 F=131. 907 X - MEAN = 3.FI05 102 COOK FGL14 A4B4C154T2 Y IELD= 68. 470

ORIGINAL DATA, INTERVALS 1,2, 3, 4 BEATING 8 308 658 1.000 CSF 718 682 416 1R5 C 01'1 CORA 11. 8 28. 4 42. 3 BULK 2. 9 2. 4 2. 1 2.8 BREAKING LENGTH 3471 7178 9174 18785 BURSTFACTOR 7. 5 19. 3 31. 2 TEAR FACTOR 121. 2 140. 3 11.E.:. 5 184.3 STIFF. (MOE ) 81799 165654 21r-r4R7 1q727:9 CONSTANTFREENESS,600, 400,200 ML CSIF BEATING 304 674 977 CONCORA 2R.5 R 48.6 BULK: 2.4 2.1 2.1 BREAK I NO LENGTH 7199 9285 18688 BURST FACTOR 19.4 30.9 TEAR FACTOR -14a 0 117.5 IA5.2 STIFF.

L I N. REGR. -BULK.. 1.6, 1.8.. . 0, 2.2 CC/GM LOG BEATING 4. 8 4.1 3.4 7 Y =-3. 571 X + 10. 528 R-9Q. = 0. 920 F= 23. 084 CSF Fsci 162 274 Y 560. 635 X +-847. 285 R-SQ. = O. 818 F= 9. 003 CONCORA ic.A, 3 57 6 48. 9 =-43. 482X + 135. 837 R-SO.= 8.985F= 128.358 BREAK I NO LENGTH 4047 12381 10716 =-8327. 965 X + 27371. 703 R-SQ. = 0. 984 F= 124. 731 BURST FACTOR 42. 1 36. 7 31. 2 =-27. 329 X + 85. 854 R-SQ. O. 990 F= 189. 475 TEAR FACTOR 108. 4 111. 7 115. = 16. 528 X + 81. 928 R-S9. = 0.176 F= 0. 428 STIFF. (MOE ) 279685 249534 219384 =-150752. 588 X + 520889. 088 R-5Q=0.955 f= 42.886 -MEAN =2. 368 103 COOK FGL15 A4B2C154T4 YIELD= 65. 520 ORIGINAL DATA,INTERVALS 1.. 2 3, 4 BEAT I NO 30174 650 lAAA CSF F-;5q 451. 225 141 CONCORA 17. 4 36.1 43.7 47.? BULK 3. 1 2.6 2.3 2.1 BREAKING LENGTH 4071 7865 9991 112q-z: BURST FACTOR 24.5 7:7. 0 TEAR FACTOR 171. 9 206. 8 132. 4 130. 3 STIFF. (MOE> 84913 162276 189304 27i:4R04 CONSTANT FREENESS,600, 400, 200 ML CSF BEATING 39 754 CONCORA - 22. 7. 37. fz: 44.9 BULK 3. A 2.6 2.2 BREAK I NO LENGTH 5147 87:45 10379 BURST FACTOR 14. -1 25.? 22. 1 TEAR FACTOR 181. 8 190. 0 131. 8 STIFF. (MOE ilatc.RF;R 168375

CONSTANT BEATING,333, 667.. 1000 PF I CSF 429 221 141 CONCORA R 47.7 BULK 2.3 2.1 BREAK I NO LENGTH 806? 101:7153 11293 BURST FACTOR 30. 3 TEAR FACTOR 199. 7 132. 3 130. 3 STIFF. (MOE ) 164850 191471 234804

L I N. REGR. -BULK, 1. 6, 1. 8, aO.. 2. 2 CC/GM LOG BEATING 4. 9 4. 3 Y -3. 036 X + 9. 782 R-SO. = 0.885 F= 15.466 CSF -17:5 RA 187 = 535. 913 X +-992. 049 R-SQ. = O. 990 F=198.736 5s.. 8 CONr.OR A 65. 59. A 46. 7 =-38.745X + 114.302 R-SO. = 0.982 F= 108. 683 BREAKING LENGTH 15140 13686 12231 10776 =-7273. 369 X + 26778. 804 R-91 = 8.998 F=964.052 BURST FACTOR 50. 44. :3 39. 34. 3 V=-26.297297 X + 92.138 R-SO. = O. 984 F=la516 TEAR FACTOR 110. 4 121. 0 131. 6 142. 3 Y = 53.169X+ 25. 291 R-SO. = 0.401 F= 1.338 STIFF. (MOE) 302257 273645 245032 216420 =-1.43062. 046 X + 531156. 500 0. 973 F=73.432 - MEAN = 2. 540 04 COOK FGL16 A4B4C3S4T4 YIELD =-*68. 970 ORIGINAL DATA, I NTER'ViRLS 1, 2, 3, 4 BEATING 0 300 650 1000 CSF 711 706 486 CONCORA 8.9 21. 8 33. 2 49. 6 BULK 3.8 2. 9 52. 2.3 BREAKING LENGTH 1271 3428 4201 4974 BURST FACTOR 5.1 18. 3 26. 9 1 TEAR FACTOR 127. 5 201. 9 166. 1 126. 1 STIFF. (MOE) 54231 149449 205375 213529 CONSTANTFREENESS,600.. 400,200 ML CSF BEATING 469 805 1166 CONCORA 27. 3 40.5 57. 4 BULK 2.7 2.4 2.2 BREAKING LENGTH 3800 4543 5341 BURST FACTOR 22.4 27. 9 30. 1 TEAR FACTOR 184.? 148. 4 107. 1 STIFF. (MOE) 176395 208990 217396 CONSTANT BEAT I NG,33.'3,667,1.000 FFIREVS CSF 685 477 299 CONCORA 22. 9 34. 0 49.6 BULK 9.8 2.5 2.3 BREAK. I NO LENGTH 3502 4237 4974 BURST FACTOR 19. 27. 0 29.1 TEAR FACTOR 198. 5 164. 2 126.1 STIFF. (MOE) 154775 205763 213529

L I N. REGR. -BULK,1. 6,1. 8,2.0.2. 2 CC/GM LOG BEATING 4. 6 4.2 3.8 3.4 Y =-2. 019 X+7.824 R-SQ.=8. 956 F= 43. 546 CSF 251 299 347 394 =238. 063 X +-ia 434 R-SQ.=0.645 F= 3.634 CONCORA 58. 0 53. 3 48. 5 43. 8 Y=-a 752X+96.039 R-S=8.866 F= 12.958 BREAKING LENGTH 6403 5933 5463 4993 V=-2349. 593 X+18161. 935 R-SQ.=8. 996 F= 444.269 BURST FACTOR 39. 8 36. 6 33. 4 2 =-16. 011 X+65.444 R-SQ.=8.989 F= 172.215 TEAR FACTOR 167. 3 165. 4 163. 5 161. 6 V=-9.494 X + 182. 445 R-SQ.= 8.832 F= 0,065 STIFF. (MOE) 290184 268637 247089 225542 =-187737. 834 X + 462565. 811 R-SQ.= 8.989 F= 184.567 X - MEAN =9.849 COOKFGL17 Fi3B5C2S3T3 YIELD= 69. 250 ORIGINAL DATA, INTERVALS 1, 2, 3,4 BEATING 300 650 1000 CSF 728 614 476 289 CONCORA 7.9 23.5 37. 0 41. 6 BULK 3.1 2.5 2.3 BREAKING LENGTH 763 3899 5032 4660 BURST FACTOR 4.7 15.2 18. 3 21. 7 TEAR FACTOR 90.5 125.7 9 119. 4 STIFF. (MOE) 72231 137600 177548 185308 CONSTANT FREENESS,600, 400,200 ML CSF BEATING 336 792 1167 CONCORA 24.9 38. 9 43. 8 BULK 2.5 2.3 BREAKING LENGTH 4014 4881 4483 BURST FACTOR 15. 5 19. 7 ""3. 4 TEAR FACTOR 124. 5 116. 1 122. 1 STIFF. ( MOE ) 141653 180702 189001 CONSTANT BEATINGS 333, 667, 1000 PF I CSF 601 467 289 CONCORA 24.8 37.2 41.6 BULK. 2.5 2.3 BREAK I NG LENGTH 4007 5014 4660 BURST FACTOR 15. 5 18. 4 21. 7 TEAR FACTOR 124. 5 114. 2 119. 4 STIFF. (MOE) 141405 177918 185308

L N.REGR. -BULK, 1. 6, 1. 8, 2. 0,2. 2 CC/GM LOG BEATING 5. 4 4.7 4.0 3.3 V -3.442 X + 10.881 R-SQ.= 0.986 F=141.535 CSF 141 222 382 = 402. 181 X +-502. 397 R-SQ.= 8.737 F= 5.595 CONCORA 62. 3 55.0 40.5 V =-36. 295 X + 120. 376 R-S. = 8.933 F= 27. 991 BREAKING LENGTH 8158 7205 5299 V=-4765.21.6 X + 15782.150 R-SQ.= O. 980 F=98.726 BURST FACTOR 28. 7 214 =-18. 059 X + 61.169 R-S. = O. 979 F= 95. 240 TEAR FACTOR 143. 5 137. 0 124. 0 =-32.486 X + 195.488 R-SQ. = O. 727F= 5. 317 STIFF. ( MOE ) 264731 ',39778 214024 188671 V =-126766. 976 X + 467558. 059 R-SO. = 8.978 F= 90.275 X - MEAN = 2. 559 106 COOKFGL18 A383C253T3YIELD 71. 180 ORIGINAL DATA,INTERVALS 1, 2, 3, 4 E:EAT I NO 300 650 1000 CSF 512 175 149 80 CONCORA 30. 6 40. 9 46.8 56.3 BULK 3. 0 2.6 2.3 2.0 BREAKING LENGTH 3101 6508 6826 8498 BURST FACTOR 10. 0 27. 0 21.4 26.3 TEAR FACTOR 146.3 133. 5 105. 0 84. 6 STIFF. (MOE) 87454 151048 216419 251824 CONSTANT FREENESS,600, 400, 200 ML CSF BEATING -78 100 278 CONCORA 27. 9 34.0 40.1 BULK 3.1 2.9 2.6 BREAKING LENGTH 22/1 4233 6255 BURST FACTOR 5.6 15.6 25. 7 TEAR FACTOR 149. 6 142. 0 134. 5 STIFF.(M0E) 70848 108589 146330

CONSTANT BEFIT I NG,333, 667,1000 PF I REV'S CSF 173 146 80 CONCORA 41. 5 47. 3 56. 3 BULK 2. 6 2.0 BREAK: I NO LENGTH F.57:8 6905 8498 BURST FACTOR 26. 4 21. 6 TEAR FACTOR 130. 8 .1134. 0 84. 6 STIFF. (MOE) 157274 218105 2.!91824

LIN.REGR. -BULK, 1. 6 1. 8, 2. 0, 2. 2 CC/GM LOG BEATING 4. 7 4. 1 3. 5 Y =-2. 9% X + 9.494 R-SQ. = 8.825 F= 9.488 CST -140 -56 28 = 421.916 X 4-815.332 R-SQ. = O. 858 F= 12. 122 CONCORA 65. 8 60. 7 55. 7 =-25. 318 X + 106.318 R-SQ. = 8.992 F=243.889 BREAKING LENGTH 10757 9723 8689 Y =-5168. 317 X + 19Ø25. 934 R-SQ. = 8. 935 F= 28.976 BURST FACTOR 33 7 30. :3 28. 0 Y =44.297 X + 56.557 R-SQ. = 8.595 F= 2.942 TEAR FACTOR 61. 3 74. 1 86. 9 = 63.989 X +-41. 040 R-SQ. O. 949 F= 37. 131 STIFF. (MOE) 326144 291991 257837 V =-170766. 955 X + 599371. 254 R-SQ.= 8.991 F= 288.571 X - MEAN = 2. 475 107 COOKFGL19 fl383C253T3 YIELD= 66. 680 'X ORIGINAL DATA, INTERVALS 1, 2, 3, 4 BEATING 0 300 650 1200 CSF 734 659 475 170 CONCORA 8.1 22. 0 35. 0 48. 7 BULK 2.7 2.3 2.1 1. 9 BREAKING LENGTH 2049 -z893 4509 545 BURST FACTOR 7.5 17.0 23. 8 28.3 TEAR FACTOR 135. 6 147. 2 112. 0 71. 1 STIFF.(M0E) 96126 183652 236433 247500 CONSTANT FREENESS,600, 400,200 ML CSF BEATING 412 785 1146 CONCORA 38.4 47.4 BULK 2. 2 2.0 1.9 BREAK: I NG LENGTH 4090 4732 5326 BURST FACTOR 19. 2 24. 9 27. 9 TEAR FACTOR 135. 9 101. 9 75. 1 STIFF. (M0E) 200576 239154 246411 CONSTANT BEAT I NG,333, 667,1000 PF IREVS CSF 641 466 281 CONCORA 35. 4 43. 7 BULK - 2.1 2.0 BREAKING LENGTH 3952 4536 5085 BURST FACTOR 17. 7 24. 0 26.? TEAR FACTOR 143. 9 110.? 86. 171 STIFF.(M0E) 188F;79 236768 243476

L I N. REGR. -BULK, 1. LOG BEATING 4. 8 Y =-4. 269 X + it 631 R-SO.= 0.941 F= 32.138 CSF Y = 672. 879 X 4-994. 1.91 R-SQ. = 0.744 F= 5.819 CONCORA 61. 6 Y =-52.197 X +145.097 R-50. = O. 933 F=27.668 BREAKING LENGTH 6760 Y =-440t 507 X + 13802. 460 R-SQ. = 0:992 F=243.530 BURST FACTOR 36. Y =-27. 946 X + 8t606 R-SQ. = O. 986 F= 140. 055 TEAR FACTOR 68. 7 87:. 8 = 75.194 X4-5t562562 R-SQ. = 8.518 F=2. 151 STIFF. (MOE) 283612 Y =-213207. 317 X + 667384. 732 R-SQ. = O. 988 F= 162. 064 X - MEAN =2. 235 108 COOKFGL20 Fi2B2C154T2 YIELD= 73. 240 X. OR 101 NALDATA NTERVALS 1, 2, 3, 4 BEATING 0 300 650 1000 CSF 678 593: 397 167 CONCORA 10. 7 24.1 50.2 64.9 BULK 3. 1 2.3 2.2 2.1 BREAKING LENGTH 919 2881 3490 3580 BURST FACTOR 5. 4 ±3.7 ±9.5 20. 0 TEAR FACTOR 99. 4 66. 6 104. 8 85.0 273594 266130 . STIFF. (MOE) 65764 175642 CONSTANTFREENESS,600, 400,200 ML CSF BEATING 275 645 950 CONCORA 23. 0 49. 8 6.-,. 8 BULK 2. 3 2.2 2.1 BREAKING LENGTH 2719 3480 3567 BURST FACTOR 13. 0 19. 4 20. 0 TEAR FACTOR 69. 3 104. 3 87. 8 STIFF. ( MOE ) 166593 272095 267201 CONSTANT BEATINGS 333, 667,1000 PF I REV'S CSF 574 386 167 CONCORR 26.6 50.9 64.9 BULK 3 2. 2 21 BREAKING LENGTH 2939 3494 3580 BURST FACTOR 14.3 19.5 20.8 TEAR FACTOR 70. 2 85. STIFF. ( MOE ) 184971 273239 266:130

L N.REGR. -BULK, 1.8 2. 0, 2. 2 CC/GM LOG BEATING 4 3.3 7 Y =-2. 897 X + 9. 056 R-SQ. = 0. 999 F= 787 CSF 168 240 311 383 Y = 358. 989 X +406. 622 R-91= a581 F= 2.768 CONCORA 71. 7 63. 3 54.8 46.4 =-42.217 X + 139.242 R-SQ.= 0. 688 F= 4.485 BREAKING LENGTH 4782 4273 3763 3254 =-2547. 275 X + 8857.875 R-SQ.= 0.985 F= 131.340 BURST FACTOR 25. 6 97,. 9 17. 5 'I =43.536 X + 47.292 R-S= 8.916 F= 21.938 TEAR FACTOR 79. 4 81. 8 24± 86. Y = 11.786 X + 60.542 R-S.= O. 110 F= 8.248 STIFF. ( MOE ) 348473 310675 272877 235080 Y =-1m-47.604 X + a0852. 687 R-SQ. = O. 881 F= 14.806 X - MEAN = 411 109 COOKFGL2l AlB3C2S3T3YIELD= 75.520

ORIGINAL DATA INTERVALS 1,2, 3, 4 BEATING 0 300 650 1000 CSF 705 572 313 205 CONCORA 8. 5 23. 2 35. 4 47. 5 BULK 3. 2 2. 5 2.2 2.1 BREAKING LENGTH 1024 2679 7-x7.0 3335 BURST 'FACTOR 4. 2 11.7 13.7 14. 3 TEAR FACTOR 83. 4 93.8 93.6 77. 4 STIFF. ( MOE ) 42523 120046 165081 190831 CONSTANT FREENESS,600, 400,200 ML CSF BEATING 237 532 1016 CONCORA 20. 1 31. 3 48.1 BULK 2.6 2.3 2.1 BREAKING LENGTH 2331 3045 3340 BURST FACTOR -10.1 13. 0 14.3 TEAR FACTOR 91. 6 93. 7 76. 6 STIFF. ( MOE ) 103725 149953 192023 CONSTANT BEAT I NG,333, 667,1000 PF I REV CSF 547 308 205 CONCORA 24. 4 36. 0 47. 5 BULK 2.2 2.1 BREAKING LENGTH 2732 3335 BURST FACTOR 11.9 13. 7 14. 3 TEAR FACTOR 93.8 8 77. 4 STIFF. (MOE) 124335 166307 190831

L I N. REGR. -BULK, 1. 6, 1.. 8, 2. 0, 2. 2 CC/GM LOG BEATING 4. 6 4. 0 "Z. 5 2. 9 Y =-Z 810 X + 9. R-SQ. = 0.966 F= 57.321 CSF 60 147 234 320 = 434.031 X +-634.466 R-SQ.= O. 852 F= it 523 CONCORA 57.? 51. 2 44.? V=-32.439 X + 109.609 R-SQ. = O. 933 F=18.595 BREAKING LENGTH 4517 4082 3646 3211 Y =-2177. 036 X +5:1.532 R-SQ. = O. 994 F= 342.106 BURST FACTOR 19. 4 17. 5 .15. 6 =-9.450 X + 34.540 R-SO. = a990 F= 207.345 TEAR FACTOR 87. 8 87. 6 87. 5 87. 3 v=-a851861 X + 89. 198 R-SQ. = O. 3 F= 0. 805 STIFF. (MOE ) 247629 221279 194929 168579 =-131748. 730 X + 458426.618 R-S. = 0.982 F= 112. 240 X - MEAN = 2. 496 110 COOKFGL22 A3B3C253T3 YIELD= 67. 360 ". ORIGINAL DATA,INTERVALS 1., 2, 3,4 BEATING 0 300 650 1000 CSF 626 349 208 106 CONCORA 18. 38. 4 46. 9 5%7. 8 ,BULK 2. 6 2.0 1.9 BREAKING LENGTH 1812 3711 3786 4235 BURST 'FACTOR 9.3 24. 0 26.7 32. 5 TEAR FACTOR 141. 7 130. '8 99. 8 99. 4 STIFF.

L I N. REGR.-BULK, 1. 6, I.. 8, 2. 0, 2. 2 CC/GM LOG BEATING 4. 7 3. 8 2. 9 2. 0 =4.608 x+1.2.1.00 R-SQ.= 8.971 F= 67.322 CSF -109 41 Y =748.098 X +-1305. 549 R-SQ. = 8.983 F= 113. 693 CONCORA 6:3. 2 58.1 47. 9 37. 8 =-58. 729 X + 149. 406 R-SQ.= 8.995 F= 366. 805 BREAKING LENGTH 5427 4718 4029 .7.301 =-3543.872 X + 11095. 614 R-SQ.=a972 F= 70.366 BURST FACTOR 41. 9 35. 4 98. 9 V=-32.784 X + 94. 269 R-SQ. = O. 987 F= 157. 853 TEAR FACTOR 75. 2 89. 4 103. 6 = 71.187 X 4-38. 728 R-SQ.= 8.881 F= 8.848 STIFF. (MOE) 348104 299472 950839 Y =-243162. 565 X + 737164. 573

R-SQ. = O. 994 F= 320. 612 X - MEAN 2. 176 111 COOKFGL23 A282C354T4 YIELD= 75. 340 ORIGINAL DATA,INTERVALS 1, 2, 3, 4 BEATING 0 300 650 1000 CSF 729 6%70*? 459 274 CONCORA 9.3 23.4 -z.5. 6 43. 2 BULK 3.2 2.2 2.1 BREAKING LENGTH 1475 3005 3501 4595 BURST FACTOR 6.2 14.8 18. 4 24. 9 - TEAR FACTOR 123. 2 143. 8 130, 8 103. 8 STIFF. (MOE ) 49493 195773 197800 241796 CONSTANT FREENESS,600, 400,200 ML BEATING 347 762 1140 CONCORA 25. 0 38. 0 46. 2 BULK 2. 2 2. 2 2.0 BREAKING LENGTH 3072 3850 5032 BURST FACTOR 15. 3 20. 4 2,. 5 TEAR FACTOR 142. 0 1'-')%9.2 93.8 STIFF. (MOE) 196047 211831 259394 CONSTANT BEATINGS 333, 667,1000 PF IREVS CSF 606 450 274 CONCORFi 24. 5 36. 0 4.2 BULK 2.2 2. 2 2.1 BREAKING LENGTH 3052 4595 BURST FACTOR 15.1 18. 7 24. 9 TEAR FACTOR 142.5 129. 6 103. STIFF. (MOE) 195966 199895 2417q*F.;

LOG BEATING =-2.791 X + 8.821 R-SQ. = 0.994 F= 345.362 CSF V = 316.468 X 4-244. 106 R-SQ. = 0.634 F= 3.462 CONCORA 49. =-26.794 X + 92. 634 R-SQ.= 8.812 F= 8.659 BREAKING LENGTH 5111 =-2405. 307 X + 8959. On R-9).= O. 860 F= 12. 265 BURST FACTOR Y =-14.280X + 58.578 R-S= 8.848 F= 18.582 TEAR FACTOR 123. Y = 241 X + 119. 984 R-5Q= 8.804 F= 8.889 STIFF. (MOE) 307749 =-166984. 390 X + 574923. 540 R-SQ.= 8.989 F= 181.932 X - MEAN = COOKFGL2 A583C253T3 YIELD= 66. 900 ORIGINALD.Frnn,INTERVALS 1, 2, 3, 4 BEAT I NG 300 650 CSF 720 615 349 CONCORA 11. 9 26.5 35. 9 BULK 3.0 2. 3 2.1 BREAKING LENGTH 2960 6341 7397 BURST FACTOR 8.6 23. 3 30. 4 TEAR FACTOR 171. 2 148. 9 111. 3 STIFF. (MOE) 79277 153891 221561 CONSTANT FREENESS,600, 400,200 ML CSF BEATING 320 583 974 CONCORA 27.0 34. 1 51. 5 BULK 2.3 2.2 2.0 BREAK I NO LENGTH 6401 7194 8715 BURST FACTOR -)3. 7 29. 1 34. 3 TEAR FACTOR 146. 7 118. 5 96. 7 STIFF. ( MOE ) 157713 208668 232066 CONSTANT BEATINGS 333, 667,1000 PFI REV.'S CSF 590 341 188 CONCORA 27.4 36.7 52. 8 BULK 2.3 2.1 2.0 BREAK I NO LENGTH 6442 7465 8821 BURST FACTOR 24.0 30.6 34. 6 TEAR FACTOR 145. 3 110. 6 95. 5 STIFF. (MOE) 160345 222196 27:2904

L I N. REGR. -BULK, 1.6, 1. 8, 2. 0, 2. 2CC/GM LOG BEATING 4. 5 3. 9 2.6 =-3.249 X + 9.724 R-SQ.= 0.969 F= 62.019 CSF 82 185 287 389 = 510.580 X 4-734.442 R-91= 0.790 F= 7.524 CONCORA 60. 1 52. 6 45. 1 37.6 =-37. 501 X+ 128. 092 R-SQ. = 8.859 F= 12.144 BREAK ING LENGTH 10794 9624 8455 7286 =-5845.738 X + 20146. 683 R-9. = 0. 984 F= 124. 499 33... 8 BURST FACTOR 44. 5 39. 1 28.4 =-26.819 X + 87.409 R-SQ. = O. 992 F= 260. 680 TEARFACTOR 74. 4 89. 6 104.7 119.9 Y = 75.968 X 4-47.192 R-91 = 0.867 F= 13.885 STIFF. (MOE ) 295798 262988 230179 197369 =-164048. ee4 X + 558274. 764 R-SQ. = 0.960 F= 47.428 X - MEAN =2. 355 1 1 3 COOK FGL24 A4B4C352T2 YIELD 76. 880 74 ORIGINAL DATA I NTERVRLS 1, 2, 3, 4 BEATING 300 650 000 CSF 7%7'8 630 430 250 CONCORA 9.la 26. 3 38. 7 43. 4 BULK 7.'") 3.6 2.2 BREAK I MG LENGTH 1664 3811 4614 6368 BURST FACTOR 5.1 5. 5 20. 7 22. 9 TEAR FACTOR 105.0 125. 1 118. 4 99. 2 STIFF. (MOE ) 71580 54264 192794 20988:3 CONSTANTFREENESS,600, 400,200 ML BERT I NG 353 708 1097 CONCORA 28. 2 39. 5 44. 7 BULK 3.4 2.3 2.1 BREAK I MG LENGTH -393-2 4906 6856 BURST FACTOR 16. 3 21. 1 23. 5 TEAR FACTOR 124. 115. 2 93. 8 ST I FF (MOE) 75044 195643 214636 CONSTANT BEATING333, 667,1_000 PF I CSF 611 421 250 CONCURR 27.5 38.9 43. 4 BULK 3.5 2.3 BREAK I NO LENGTH 3888 4697 F.368 BURST FACTOR 16.0 20.8 22. 9 TEAR FACTOR 124. 5 117. 5 99. *, STIFF. (MOE) 67457 193608 209888

L I N. REGR. -BULK, 1. 6, A_ 8, 2.0, 2. 2 CC/GM LOG BEATING 3. 3 3. 1 2.9 2.7 Y =-1. 012 X+4. 923 R-SQ.= 8.244 F= 8. 644 CSF 178 232 287 Y=272.389 X+-257.953

R-SQ.= 8.762 Fmt6.488 CONCORA 49. 9 46. 5 43.i 39.8 =-16.851 X+76.828 R-S.= 8.568 F 2.543 BREAK I NG LENGTH 6587 6181 5774 5368 Y =-2030. 734 X+9835. 915

R-SQ.= 0.504 F= 2.032 . BURST FACTOR 25. 8 24. 2 22.6 21.0 V=-8.016 X+38.623 R-SQ.= 8.473 F= 1.797 TEAR FACTOR 100. 9 102. 7 104. 5 106. Y = 9. 065 X + 86. 367 R-SQ.= 8.269 F= 8.735 STIFF. (MOE) 274049 250736 227423 204110 =4.16565. 691 X + 468554.119 R-SO.= 8.975 F= 78.278 X - MEAN = 2. 817 COOKFGL25 Fi383C255T3 YIELD= 66. 190 X. ORIGINAL DATA INTERVALS 1. 2, 3, 4 BEAT I NO 0 300 650 100121 CSF 71719 41'9 234 CONCUR Ft 10. 3 28. 2 34. 4 43. 0 BULK 3. 1 2.3 "7. 2 2. 3 BREAK I MG LENGTH 1566 3683 4300 4664 BURST FACTOR 7.4 20. 4 5 32. 8 TEAR FACTOR 135. 6 139. 6 133. 3 144. 3 STIFF. (MOE) 81881 188052 154423 192606 CONSTANT FREENESS,600, 400,200 CSF BEATING. 27121 717 1058 CONCORA 26. 4 36.0 44. 4 BULK 2.4 2. 2 2. 3 BREAKING LENGTH 3473 4369 4724 BURST FACTOR 19. 1 3 34. 4 TEAR FACTOR 139. 2 135. 4 146. 1 STIFF. (MOE) 177523 161687 198939 CONSTANT BEATING,333, 667,1.000 PF IREV S CSF 574 429 234 CONCORA 28. 8 34. 8 43.0 BULK 2.2 BREAKING LENGTH 3742 4317 4664 BURST FACTOR 291. 7 0 0 TEAR FACTOR 139. 0 133. 8 144. 3 ST I FF MOE 184849 156241 192606

L I N. REGR. -BULK, 6, 1. 8, 2. 0, LOG BEATING 5. 1 4.4 =-3. 459 X + 10.684 R-SQ.= 0.978 F= CSF 179 7.05.7 Y = 361.250 X+-398.612 R-SQ.= 0.498 F=1.984 CONCORA 55. 9 49. 7 =-31.11.6 X + 106.730 R-SQ.= O. 7 F= 8.358 BREAKING LENGTH 6435 5770 5105 4440 Y =-3324. 728 X + 11754.624 R-S8.921 F= 23. 244 BURST FACTOR 40. 6 36. 1 V=-22.571 X + 76. 706 R-SQ. = 0.736 F= 5.576 TEAR FACTOR 141. 5 140. 7 140. 0 =-3.793 X + 147. 546 R-SQ. = 0.098 F= 0.219 STIFF. (MOE) 256397 2824 209252 185680 =-117861. 551 X + 444975. 062 R-SQ. = 8.849 F= 11.211 X - MEAN :=2. 4 115 COOKFGL26 A3B3C2S1T3 YIELD= 68.450 ORIGINAL DATA,I NTERVALS 1, 2, 3, 4 BEATING 300 650 1000 CSF 625 374 7-z28 CONCORA 11. 0 21. 5 40. 0 48. 2 BULK 3.0 2.7 2.5 2.5 BREAKING LENGTH 1563 2856 3609 3743 BURST FACTOR 6.5 14. 0 17. 1 17. 4 TEAR FACTOR 124. 1 168. 9 126. 8 1.17. 8 STIFF. (MOE) 76422 142052 221750 198651 CONSTANT FREENESS,600, 400, 200 ML CSF BEATING 614 1974 CONCORA 23. 3 38. 1 7-1. 0 BULK 2. 7 2.5 2.5 BREAKING LENGTH 3531 4116 BURST FACTOR 14. 4 16.8 18.4 TEAR FACTOR 164. 7 131. 2 92. 8 STIFF. (MOE) 149990 213494 134376 CONSTANT BEATING, 333, 667, 1000 PF I REV S CSF 601 372 CONCORA 40.4 48.2 BULK 2.7 2.5 2.5 BREAK: I MG LENGTH 3615 3743 BURST FACTOR 14. 3 17.1 17.4 TEAR FACTOR 164. 8 126. 4 117. 8 STIFF. (MOE) 149642 2206591 198651

L I N. REGR. -BULK, 1. 6, 1. 8, 2.a.2. 2 CC/GM LOG BEATING 7. 9 6. 8 5.? 4. 7 =-5.349 X + 16.431 R-Sa=a 884 F= 1.5. 205 CSF -246 -108 31 169 = 692.423 X+-1353.895 R-S.=a F= 1.5. 920 CONCORA 101. 6 88.5 75.3 62.1 Y =-65.918X + 297. 115 R-92 = 8. 912 F= 29. 603 BREAKING LENGTH 7321 6513 5706 4898 =-4037.914 X + 13781.500 = 0.987 F= 151.632 BURST FACTOR 35. 7 31. 7 27. 6 23. 6 V=-2a262262 X + 68.146 R-S. = O. 965 F= 54. 580 TEAR FACTOR 116. 5 119. 8 123. 1 126. 4 =16.512 X + 90.046 R-S= 0.030 F= 8.863 STIFF. (MOE) 443192 390903 338615 286326 =-261443.371 X + 86150.1.486 R-SQ.= 0.983 F= 112.753 X - MEAN = 2. 684 COOKFGL27 Fi2B4C354T2 YIELD= 78. 750 ORIGINAL DATA,INTERVALS 1 2, 3, 4 BEATING 0 300 650 1000 CSF 715 591 430 197 CONCORA 10. 8 9'3% 1 3/. 5 48. 8 BULK 3. 2 2.5 2. 3 2.2 BREAKING LENGTH 1296 3239 3595 BURST FACTOR 6.'I" 13. 7 15.5 19. 0 TEAR FACTOR 132. 0 101. 3 87. 5 STIFF. ( MOE ) .58204 119581 175701 186307 CONSTANT FREENESS,600, 400,200 MLCSF BEATING 278 695 995 CONCORA 21. 3 33. 8 48. 6 BULK 2. 6 2.3 BREAKING LENGTH 2529 3285 3590 BURST FACTOR 13.2 15.9 19. 0 TEAR FACTOR 129. 1 99. 5 87. 7 STIFF. ( MOE ) 115126 177067 186170

CONSTANT BEATING, 33 , 667,1000 PF I REV CSF 576 419 197 CONCORA 23. 0 32. 4 48. 8 BULK s".5 2.2 BREAK I MG LENGTH 2684 3256 3594 BURST FACTOR 13. 9 15. 6 19. 0 TEAR FACTOR 129. 1 100. 6 87. 5 STIFF. (MOE) 124926 176206 186307

L I N. REGR. -BULK.. I. 6, 1. 8.. 2. 0, 2. 2 CC/GM LOG BEATING 4.3 3.7 3.1 =-3.833 X + 9.885 R-91. = 8.965 F= 55.394 CST* 66 154 242330 = 439. 484 X +-637. 323 R-S.= 0.792 F= 7.635 CONCORA 59. 0 52.5 46.1 39.6 Y =-32.274 X + 118.614 R-SQ. = 8.827 F= 9.554 BREAKING LENGTH 4802 4357 3912 3467 =-2224.971 X + 8361.971 R-S= 8.994 F= 335.692 BURST FACTOR 24. 9 20. 1 17. 8 =-1t849 X 4. 43.824 R-SQ. = O. 986 F= 136.865 TEAR FACTOR 104. ,F4 104.5 104. 2 103. 9 V=-i648 X + 107. 481 R-SQ.= 0.881 F= 0.083 ST I FF. ( MOE ) 255428 230057 204686 179315 =-126854. 942 X + 458396. 271 R-91 = 8.951 F= 38.486 X - MEAN =2.550 COOKFGL28 A482C352T4 YIELD= 71. 980 ORIGINAL DATA,INTERVALS 1, 2, 3, 4 BEAT I MG 0 300 660 1000 CSF 703 655 345 145 CONCORFI 9.8 28.2 43.1 46. 4 BULK 3. 8 2.4 2.0 2.1 BREAK I MG LENGTH 1092 3857 5006 5133 BURST -FACTOR 4.3 21. 5 29. 0 26. 0 TEAR FACTOR 94.0 129. 5 92. 6 82. 7 STIFF. (MOE ) 50960 207005 286857 255732 CONSTANT FREENESS,600, 400,200 ML CSF BEATING 364 596 907 CONCORA 30. 40. 5 45. 5 BULK 2.3 2.1 2.1 BREAK I MG LENGTH 4061 4802 5098 BURST FACTOR '72. 8 27.6 26.8 TEAR FACTOR 123.Ci 99. 1 85. 4 STIFF. (MOE) 221172 272690 264291 CONSTANT BEAT I NG,333, 667,1000 PF I REV'S CSF 626 341 45 CONCORA 29. 6 43.2 46.4 BULK: 2.3 2.0 2.1 BREAKING LENGTH 3964 5009 5133 BURST FACTOR 22. 2 28. 9 26. 0 TEAR FACTOR 126. 1 92. 4 82. 7 STIFF. (MOE) 214399 286247 255732

L I N. REGR. -BULK, 1. 6, 1. 8, 2. 0, 2. 2 CC/GM LOG BEATING 3. 7 3. 4 3.1 2.7 Y =4.661 X + 6.373 R-SQ. = 0.991 F= 219. 716 CSF 244 288 33:2 376 Y = 228. 013 X +407. 570 R-SQ. = O. 488 F= 936 CONCORA 50. 3 46. 6 42. 9 39. 1 =-18. 666 X + 80. 198 R-S 0.878 F= 14.444 BREAKING LENGTH 5951 5510 5070 4629 Y =-2203. 893 X + 9477. 426 R-SQ. 8.971 F= 66.632 BURST FACTOR 33. 1 30. 5 sv7.9 25. 2 =43.042 X + 53. 937 R-SQ. = 8.984 F=12t949 TEAR FACTOR 100. 8 100. 6 100. 4 100. 1 Y 097 X + 122.556 R-SQ.= 0.082 F= 8.084 ST I FF. ( MOE ) 321935 297300 272s;64 248029 =-123176. 364 X + 519017. 137 R-9). = O. 974 F= 73.89'3 X - MEAN = 2. 589 118 A3B3C2S3T3 YIELD= 68. 080 X.

ORIGINAL DATA INTER VtFIL.S;1,2343, 4 BEATING 0 30ci 650 1000 CSF 701 604 210 CONCORA 12. 9 26. 4 40. 7 45. 1 BULK 2. 7 2.2 2.0 2.13 BREAKING LENGTH 1823 2954 4537 4620 BURST FACTOR 8.5 29. 8 28. 5 32. 0 TEAR FACTOR 166. 7 162. 4 107. 0 105. 2 STIFF. (MOE) 100098 209776 248334 919755 CONSTANT FREENESS,600, 400,200 !IL BEATING 305 1028 CONCORA 26. 6 37.2 45.5 BULK 2.2 2.1 2.13 BREAKING LENGTH 3963 4393 4627 BURST FACTOR 99. q 27.1 32.3 TEAR FACTOR 161. 6 120. 7 105. 1 STIFF.(MOE) 210345 238801 217432 CONSTANT BEATING, 333,667,1000 PFIREV'S CSF 578 327 210 CONCORA 27. 7 40. 9 45. 1 BULK 2. 2 2. 0 2. 0 BREFiK I NO LENGTH 4010 4541 4620 BURST FACTOR 23. 4 28. 7 32. 0 TEAR FACTOR 157. 106. 9 1135. 2 STIFF. (MOE ) 213448 246973 219755

LIN. REGR. -BULK, 1. LOG BEATING 4. 9 Y-4.381 X + 11953 R-92. = 8.971 F= 67.859 CSF 47 = 633. 214 X 3-965. 881 R-S.= 8.756 F= 6.193 CONCORA 60. 5 Y =-44.647 X + 131.931 R-SQ. = O. 920 F= 22. 882 BREAKING LENGTH 6448 Y =-4143.547 X + 13877.191 R-SQ. =O. 993 F= 279. 159 BURST FACTOR 44. 3 Y=-32.629 X + 96.535 R-SQ.=9.979 F= 93.175 TEAR FACTOR 77. 1 = m.9136X +-65. 125 R-S.=0.685 F= 4.341

STIFF. tr.MOE > 326645 286291 Y =-201778. 794 X + 649478. 343 R-Sa= 8953 F= 40.391 X - MEAN 119 COOKFGL30 F12B4C154T4 YIELD= 68. 080 ORIGINAL DATA, INTERVRLS I, 2, 3, 4 BEATING 0 300 650 1000 CSF 735 604 349 248 CONCORA 8. 8 21. 8 38. 4 43. 8 BULK 4.1 3.0 2.5 2.4 BREAK I MG LENGTH 887 3250 3973 3839 BURST FACTOR 4. 1 11. 9 18. 7 ".)1°. 3 TEAR FACTOR 100. 6 155. 2 137. 5 128.? STIFF. crioE) 44295 13.52421 158731 188364 CONSTANT FREENESS, 600, 400, 200 ML CSF BEAT I NG '305 580 1166 CONCORA 22. 1 3.5. 0 46. 4 BULK 23 26 BREAKING LENGTH 3251 3829 3775 BURST FACTOR 12. 0 17. 3. 25. 5 TEAR FACTOR 155. 0 141.-1 124. 5 ST I FF. < MOE ) 135610 154033 202447 CONSTANT BEATING, 333, 667, 1000 PF I REVS CSF 580 344 248 CONCORA 23. 4 38. 6 43. 8 BULK -.". 9 25 24 E:REAKING LENGTH 3319 3967 3839 BURST FACTOR 12. 6 18. 9 21% --z TEAR FACTOR 152. 5 137. 1 128. 7 STIFF. (MOE) 137479 160142 188364

L N. REGR. -BULK, 1_ 6, /.. 8, 2. 0, 2. 2 CC/GM LOG BEATING 4. 6 4. 2 7.9 V=-i786 X + 7.427 R-SQ.= 0.975 F= 77.281 CSF 113 Y = 265. 657 X .1-312. 335 R-SQ.= 8.836 F= 10. 294 CONCORA 55. 6 51. 7 =-19.625 X +87.824 R-SQ. = O. 905 F= 19. 012 BREAKING LENGTH 5554 5187 4820 4452 =-1836.458 X + 8492. 462 R-91. = O. 979 F= 91. 639 BURST FACTOR =-18. 351 X + 45. 522 R-SQ. = 0. 921 F= 23. 209 TEAR FACTOR 158. 7 V=-28.148 X + 190. 898 = 8.467 F= 753 STIFF. (moE ) 2437:06 =-79885.687X + 371123. 346 R-SQ. = O. 987 F= 149. 850 X - MEAN = 2. 99:3