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    1 Comtrol of Portland Cement Quality

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    Control of Portland Cement Quality By Clyde W. Moore PCA. Portland Cement Association $520 016 Orchard Road Skokie, Minas 50077-1083, 847.966.6200 Fax 847.966.9781 ve coment org ‘An oganzatongl cement companies to improve and etond the usage potand coment and conte through market evelopment, enginoerin,rsoarch, ‘education, anaiiicatfairs work. contol of Fortand Cement Quality Keywords: cement chemistry, cement manufacturing, cement production, cement testing, control chats, ‘quality control, statistical process control Reference: Moore, Clyde W., Control of Portland Cement Quality €B121, Portiand Cement Assocation, Skokie, linois USA, 2007, 172 pages. ‘About the Author: Clyde W. Moore retired from Lone Star Industries as Vice President of Production for ‘the Pyrament® Division. A long-time member of ASTM international, Mr. Moore is an Honorary Member cof Committee C-01 on Cement and an Honorary Member of Committee €-02 on Emission Spectroscopy ("ow deactivated). Mr. Moore's career spans more than forty years serving in virtually every poston of quality assurance responsibilty within cement manufacturing. Portland Cement Assocation ("PCA") isa not-for-profit organization and provides this publication solely forthe continuing education of qualified professionals. THIS PUBLICATION SHOULD ONLY BE USED BY QUALIFIED PROFESSIONALS who possess all equired license(s), who are competent to evaluate the significance and limitations ofthe information provided herein, and who accept total responsibilty for the application of this information. OTHER READERS SHOULD OBTAIN ASSISTANCE FROM A QUALIFIED PROFESSIONAL BEFORE PROCEEDING. PCA AND ITS MEMBERS MAKE NO EXPRESS OR IMPLIED WARRANTY WITH RESPECT TO THIS PUBLI- CATION OR ANY INFORMATION CONTAINED HEREIN. IN PARTICULAR, NO WARRANTY IS MADE OF MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE. PCA AND ITS MEMBERS DISCLAIM ‘ANY PRODUCT LIABILITY (INCLUDING WITHOUT LIMITATION ANY STRICT LIABILITY IN TORT) IN CONNECTION WITH THIS PUBLICATION OR ANY INFORMATION CONTAINED HERENN. Cover photo credits: WARNING: Contact with wet (unhardened) concrete, HAG-G fully automated fusion ‘mortar, cement, or cement mocures can cause SKIN IRITA- machine courtesy of Herzog Auto- TION, SEVERE CHEMICAL BURNS (THIRD DEGRE®, or SERI- mation Corp, Cleveland, OH (OUS EVE DAMAGE. Frequent exposure may be associated ‘with iitant andlor allergic contact dermatitis. Wear water- proof gloves, a long-sleeved shir, fullength trousers, and proper eye protection when working with these materials. f (©2007 Portiand Cement Assocation YoU have to stand in wet concrete, use waterproof boots that are high enough to keep concrete from flowing into them. Wash wet concrete, mortar, cement, or cement ‘matures from your skin immediately. Flush eyes wit clean . water immediately after contact. Indirect contact through ‘Allright reserved. No part ofthis Clothing can be as serous as direct contact, so promptly book may be reproduced in any form rinse out wet concrete, mortar, cement, or cement mixtures without permission in witng from from dothing, Seek immediate medical attention f you the publisher, ecept by a reviewer have persistent or severe discomfort ‘who wishes to quote bref passages in a review written for inclusion in a magazine or newspaper. TABLE OF CONTENTS PREFACE... oo see Mi FOREWORD. vil ‘ACKNOWLEDGMENTS. ix T INTRODUCTION... seectes v 1.1, What is Quality? 1 1.2. Whatis Control? 2 1.3. The Process. 2 1.4. The Raw Materials 3 2 ELEMENTS OF A QUALITY CONTROL PROGRAM 7 2.1. A Corporate Policy on Quality 7 2.2, Sources of Current Specifications 8 2.3. Competitive Conditions. : ror ~. B 2.4. Functional Quality Control. 5 5 oe 2.5. Chemical Analysis and Physical Testing — Precision and Accuragy.....2.26.ccc.. 18 2.6.50 9000 - Quality Management and Quality Assurance Standards. a 2.7. Quality is Everybodys Business... a 2.8, Summary eee see DB 3 CATALOG OF CHEMICAL CONTROL PARAMETERS : iB 3.1. Choice of individual Oxides as Control Parameters n 3.2. Choice of Compound Composition as Control Parameters 2» 3.3. Other Moduli in Common Use as Control Parameters 30 3.3.1. The Hydraulic Modulus 30 3.3.2. The Alumina Modulus. 30 3.3.3. The Silica Modulus . : 30 3.3.4, The Lime Standard = 3l 3.3.5, The Lime Saturation Factor... ..- ce a ol 3.3.6. The Lime Factor con ce . al 3.4. Choice of Lime Facto, Silica Ratio, and AVF Ratio as Control Parameters 32 3.5. Choice of Lime Saturation Facto, Silica Rati, and AF Ratio for Control a) Comal of Prtand Cement Quay 3.6. Choice of Hydraulic Modulus, Silica Ratio, and AVF Ratio for Control BY. SUMMA. eee ee eee eeee reer ‘4. HOW DATA BEHAVE — DESCRIPTIVE STATISTICS. 4.1. Descriptive Methods . 4.1.1. Definition of Sample and Population, 4.1.2. Measures of Central Tendency A Mean, 8. Median .. C. Mode D. Other Measures of Central Tendency. 4.1.3, Comparison of Measures of Central Tendency 4.1.4, Measures of Dispersion A Range. B. Average Deviation C. Standard Deviation D. Coefficient of Variation 4.1.5. Graphical Presentation of Large Samples of Data... 4.2. The Theoretical Frequency Distributions... 4.2.1. The Normal Distribution . 4.2.2. Chi Squared Distbution (32) 4.2.3. The Poisson Distribution ... 4.2.4, Other Distributions .. 4.3. Presenting Data to Convey the Maximum Information. 4.4, More About the Range and Paired Samples. 4.4.1. Use in Duplicate Tests on a Single Sample. 4.4.2. Single Tests on Paired Samples 4.43. Moving Range for Data in Order of Production... 45, Summary. '5 HOW DATA BEHAVE — INFERENCE AND PREDICTION 5.1. Distribution of Sample Means 5.1.1. Sampling From a Normal Distribution .... 5.1.2. Sampling From a Non-normal Distribution 5.1.3; Confidence Limits for Means 5.2. Hypothesis Tests 5.2.1. Erors in Decisions 5.2.2. lnferences About Means 5.2.3. Inferences about Variances 5.2.4. Confidence Limits for Variances and Standard Deviations 5.3. Summary. . 6 THE DEVELOPMENT AND USE OF QUALITY CONTROL CHARTS, . 6.1. How Processes May Behave, 6.1.1. When the Process Average is Not Controlled ... 6.1.2. Process Capability. 6.1.3. When the Process Variability is Not Controlled 6.2. Determining Piant Standards and Limits 6.2.1. Based on Individual Tests 6.2.2. Based on Tests Divided into Rational Subgroups 6.2.3. individual Values or Subgroups? . 6.3. Criteria for Action Based on Quality Control Charts. 6.4. Applications 6.4.1. Kiln Feed Control 6.4.2. Clinker Control 6.4.3. Control of Finish Grinding. 6.5. Summary. . 7 SOLVING FIELD PROBLEMS. 7.1, Developing the Investigative Approach .... 7.2. Results of the Investigation 7.3. Review of the Findings and Revision ofthe Investigation. 7.4, Conclusions and Recommendations 75. Summary. 8 INSTRUMENTATION . 8.1. Keay Equipment 8.1.1. al Instruments 8.1.2. Physics ofthe Analytical Problem 8.1.3, Progress in Research... 8.1.4 Progress in Sample Preparation. m4 m 6 6 7 B aI at 8 3 6 88 8 93 95 106: = 108 +108 108 108 = ind 1B 114 114 116 117 117 121 11 a2 122 124 125 onto of Prtand Cement Quay 8.1.5, Standard Reference Materials 8.1.6. Need for Correction Factors 8.1.7. On-steam X-ray Instrumentation 8.2. Neutron Activation Analysis, 8.2.1. Discovery and Properties of Neutrons 8.2.2 Production of Neutrons. ... 8.23. Discovery of Californium 252 ..........+ 8.2.4. Applications in the Cement industry 8.2.5. Orstream Neutron Activation Instrumentation 8.2.6. Third Evolutionary Development in Neutron Activation Instruments. 8.3. Additional Automated Systems... 8.4. Laboratory Instruments . 8.4.1 ame Photometry. 8.42. Atomic Absorption . 85. Choosing an Instrument 86. Safety. 8.7. Summary. Appendix A... Appendix 8 ‘The Augmented Matrix What itis, and how to use it - with examples. 81: What itis 82: How to use it 3: An example from the text. REFERENCES ‘ASTM STANDARDS INDEX vi 127 127 129 130 130 2130 131 131 132 13 + 133 13g 2135 2135 136 = 136 136 139 45 147 147 a7 a7 147 149 153 155 PREFACE ‘An objective of process control is continual improvement. The success of Dr. W. Edwards Deming with statistical process control, toward that end, is legendary history. This book em- pphasizes that approach, But itis nota statistics book ~ you can find dozens of those on the library shel. ts @ book on controling qual in portland cement. Statistical process control is @ means to an end. It requires a knowledge of how data behave, and how to extract al the information from ths principle: Persistent attempts at oversimpli- cation of the subject isnot nearly as productive as equivalent effort directed toward a sound Understanding of the fundamentals. That principle is applied in te lat chapter on instrumen- tation as well a to those on statistic. ‘A key feature of this book i that it uses examples of data taken from plant record; the results ‘of test which most ears work wth on a daily basis. Computer simulations are also used here they can demonstrate special characteristics of data more efficiently. Those cases are properly identted. Frequently all the information we have on a problem, or a special situation, is contained in the data. The more information we can extract from the data, the better we can ‘manage the problem, ‘A brief description of the manufacturing process and the raw materials is also included simply ‘san outline for those already familiar with it, and who speak the language of the cement plant laboratory. The essential elements of a quality control program are identified and described. There are choices of chemical control parameters, Al of those in common use today are described, and the relationship between the contol parameters and the compound com- position is derived. Methods of designing a four-component mix to meet selected chemical conditions ae demonstrated. ‘Then instrumentation is described. X-ray instruments for chemical analysis have dominated both the laboratory and on-stream process control for decades. A replacement for process contol Using neutron activation analysis has emerged in the past twenty years, and has demonstrated its effectiveness. Laboratory instruments using flame emission and atomic absorption spectrom- etry are reviewed. Contra of Portand Cement Quality Ler: FOREWORD “3 > Clyde Moore's Control of Portland Cement Quality provides a practical approach tothe application of statistical methods for quality control in the manufacture of cement. tis a ‘unique and valuable addition to the Portland Cement Association’ series on hydraulic cement manufacturing. ~ ‘A key element ofthe book is the concept of functional qualty control, which sets the stage for 2 qualty program that not only recognizes the elevance of product specifications and quality requirements for clinker and cement, but also performance characteristics required in the marketplace. The discussion of implementation of functional quality contol through an under- : standing of the effects of chemical constituents on cement composition and performance, and the use ofthese constituents as control parameters, brings the concept to reality. Moore’ use cof both real and simulated examples representing actual plant conditions provides the reader with specific guidance and direction, ‘The author’ thorough description of statistical methods along with lar, real-world examples ‘rom cement plant operations makes this an extremely useful book ~of interest to anyone responsible for making uniformly high-quality cement. tis an important reference for plant managers, and corporate and plant quality department personnel. t wil also be of interest to cement users and specifiers, and the academic community. ‘Clyde Moore has created a fundamental resource for the cement industry ‘Anthony €. Fiorato CTUGroup ACKNOWLEDGMENTS First, | wish to express my appreciation and my thanks to Lone Star Industries, Inc. and to Roger Campbell, its Executive Vice President, for permission to use data from reports | had prepared earlier for internal use. The data were contributed by each plant laboratory. They are part of this, and | thank each individual for their contributions: all wre fiends. Richard Bohan, Steven Kosmatka, Paul Tennis, Michelle Wilson, and Connie Field of the Portland Cement Association and Tony Fiorato and Javed Bhatty of CTL Group have offered ‘encouragement and editorial assistance. Clyde Moore, Jc rendered editorial assistance and contributed to Section 2.6 on 1S0 9000. Thanks to all! My family has been very patient and supportive. My sincere and humble thanks go to each of them, and this book is dedicated to them colectively (Clyde W. Moore Houston, Texas ‘To my family: Py Clyde Jr, Sandra Barry, Kristin, Jennifer, Kevin Photomicrographs of hardened Aspdin cement paste obtained from samples produced about 1848, Although the unhydrated portland cement clinker particle are far from identical to those of modern production, they clearly contain, among other phases, the our principal phases typical of portland cement 1 INTRODUCTION he first patent on “portland cement” is over 180 years old. A bibliography of publications currently a ‘on portland cement would be impressively long. However, the number of items devoted exclusively to control of quality in the manufacturing process would be quite short. Entries on the chemistry of cement ‘would constitute a substantia fraction of the list. Moreover, the quality of portland cement is dictated not only by chemical composition but also by the specific surface (fineness) ofthe finely divided finished product, the particle size distribution, the control of the production. This book is about making adjustments in the manufacturing process for portland cement in order to contol the quality of the product. The fist order of business isto create a fairly ‘good idea of what quality is, and how to approach the process of controling it. A general description of the manufacturing processes will be required. Qualty contol is a major item inthe cement plant budget. Personnel and laboratory equipment are major investments ‘A corporation’ reputation may rest on the perception within the construction industry of the quality of ts products. The objective ofthis document isto outline a qualty contro pro- ‘gram which wil yeld the most effective use of manpower and equipment and improved uniformity ofthe product. ‘The daily tasks of the laboratory staff consist largely of collecting samples periodically at fxed points inthe process, conducting tests on those samples, interpreting the results, and making decisions on whether changes need to be made at the numerous places where controls exercised. Some Points in the process may be sampled a dozerror more times per day with tess run each time — itis a 24-hour per day ‘monitoring operation. The quality contol plan must identify ‘hat properties willbe tested, the frequency, where the samples will be collected, what test will be run, andthe procedure for making decisions and implementing changes. Before progress can be made, some basic questions must be answered, agonmane Gana UF HE UHR, He HELL CAF De QUT different for different sources and classifications of coal Sulfur compounds and chlorides wil influence the state Of the alkalies. Alkali sulfates are less volatile than alkali chlorides at kiln temperatures. Therefore, a substantial ‘amount of sulfates may be retained in the clinker weile € substantial amount of chlorides may be lost with the exhaust gases and dust. inkering, and the additions interground with the clinker in the final stage of 1.1. What is Quality? In considering a dissertation on qualty control itis appro- priate to consider at an early stage the question “What is quality?” Many tert on the subject do not attempt to define quality, as though the definition were intuitively obvious. Perhaps its. A general perception of quality sas a synonym for “general excellence." That concept may date back to the time of Aristotle. Does that imply that quality can only be Positive or good — never poor? It does, then itis in err. In many senses quality ike beauty is in the eyes of the be- holder: inthe case of cement, in the eyes ofthe customer. Since this text will be considering the control of quality, a definition aimed atthe qualty ofa product is appropriate. ‘The first text using statistics as a tool in quality contol was by Walter A, Shewhart and was appropriately titled, "Economic Control of Qualty of Manufactured Product.” The author devotes Chapter IV tothe “Definition of Qualty.* The genius of Or, Shewhart shines like a beacon when his, Work is compared to current texts, and the reader realizes hhow much of the technology he had nailed down in that fist edition. (Shewhart 1931, pages 37-57) In this case, quality shall be considered the set of characteris- ties which distinguish an object fom similar items: ie, one cement sample from another. There fs a need to further restic the st to quantitative, measurable, characteristics to eliminate the aesthetic properties imparted by the cement to concrete such a texture, an feel. There wil always be 4 Include ful, calcium carbonate component, an aluminum ‘oxide component, a silicon dioxide component, a ferric oxide component, anda calcium suifate (gypsum) component, plus the interground additions. In many plants the aluminum ‘oxide component, slicon dioxide component, and the ferric ‘oxide component will be supplied largely from a single mate- Tal such as day or shale. An additional high slica material such as sand, and a high iron material suchas iron ore may be needed to give adequate chemical contro. Recently a ‘trend has developed toward using cement kins to recycle a variety of waste materials, some of which may be considered hazardous. Examples of materials commonly used for fuel ‘Table 1.1 Examples of Commonly Used Materials for Fuel and Raw Mix Components Fuel ‘A. Coal, may include anthracite, bituminous, subbituminous, and perhaps lignite. A compromise between price, ash content, and heating value must be made 3. Natural gas oil Petroleum coke Recycled organic hydrocarbons Recycled solids such as sawdust, automobile tre, processed municipal solid waste, etc Calcium carbonate component ‘A. Limestone containing CaCO inthe calcite crystal structure is the most| common 8. Ooltc aragonite containing CaCOs in the aragonite crystal structure is avilable from marine deposits at some coastal locations C. Marl, and shells from deposits which may be recent in geological terms ‘Aluminum oxide component A. Clay B. Shale ‘C. Waste products from aluminum refining D. Bottom ash (also used as source of silica) Silica component ‘A. All of the natural sources of alumina contain significant amounts of silica B. Sand and sandstone C. Bottom ash Iron oxide source ‘A Iron ores (principally hematite) B. Waste products high in iron content and for raw mix components are listed above, including 2 _—_adtional components are used, improvised strategies for few examples of the waste materials blending them with one of the other components may be required. Cement plants may have storage and metered feed systems for three or four raw mix components. A frequent combina- A quality control program to unite these independent tion indudes three components: imestone, shale, and ether materials into a product favored by the construction industry sand or iron ore. Occasionally all four will be required. When is the primary objective. The production of portland cement requires strict adherence to quality procedures throughout the entire manufacturing process 2 ELEMENTS OF A QUALITY CONTROL PROGRAM hen Joseph Aspdin conducted his experiments which led to the first patent of a hydraulic binder called “Portland Cement” in 1824 he may have been the last to make the product without quality standards. He must have enjoyed the luxury of defining the quality of the product as he proceeded. But even he had to consider some observations from earlier experimenters. John Smeaton, an en: ned to rebuild the Eddystone Lighthouse off the coast of Cornwall, England in about 1756 had already ‘observed that some combinations of lime-bearing materials had hydra commi Furthermore, Smeaton made the important discovery thatthe better limes for that purpose were those containing a con- siderable proportion of clayey materials. He even observed that better results were obtained when using as litle water as possible in mixing the ingredients into the two-inch sized balls he used for testing, Those observations must have been guidelines for Aspdin’s research, Aspdin’s cement specifications called for a “specific quantity” oflimestone and a “specific quantity” of cla, leaving the impression that the actual quantity must depend on the prop- erties ofthe limestone and the clay. Once the dnker was burned, the description contained in one of his letters says that he made the cement from a mixture of "tender and hrard-bumed clinker.” tis clear, therefor, that limitations on composition and the burning process were established eaty, and remain with us. Bogue, Lea, Gooding and Halstead provide additional detailed descriptions of the early develop- ment of porland cement. 2.1. A Corporate Policy on Quality Each cement manufacturing company should have a policy Con the quality of its products. The policy may be broad and very general. It may acknowledge the effect of product quality on corporate profitability. it may contain a statement ‘of intent to supply cement meeting all applicable specifica: tions. it may direct that quality standards shall be estabished yeer who had been properties and others did not. for each product, and periodicaly reviewed, but revised only with the approval ofthe responsible staff office, The policy may address the procedure for handing complains. must designate the corporate staff officer responsible for quality and thei ines of authoxity to appropriate field units charged with the task of assuring that quay standards are met Periodic reviews of results should be conducted by senior ‘management to ensure that both the test results and the business results expected ofthe policy are being achieved ‘The corporate policy on quality should be available to all corporate personnel ‘Thomas Peters and Robert Waterman, Jt, in their book In Search of Excellence: Lessons from America’s Best-Run Companies, conducted interviews at 62 companies. Some ‘manufactured products, and some provided a service. They found a common thread devoted to quality, service, and reli- ability in the companies they deemed excellent. The employ- 5 of those companies, from the chairman to the laborer, ‘were indoctrinated in devotion to the customer’ needs. \W. Edwards Deming states, “Quality contra, to be successful in any company, must be a learning process, year by year, top management leading the whole company...There are no shortcuts.” (Deming 1982, page 75) Quality begins with the corporate policy. The search for auality never ends Cont of Ford Cement Quality 2.2, Sources of Current Specifications ‘The cement chemist of today must be familiar primarily with ASTM C 150, Standard Spectcation for Portland Cement, and any revisions as they are approved and published, The current issue is ASTM C 150-05, the suffix designating the year of the latest change in the specication, Itis under the jurisdiction of ASTM Committee C01 on Cement which was ‘organized in 1902. Five major types of cement are specified, designated Type | through Type V, and there are ai-entrain- ing vesions of tree of them, designated Type IA, A, and WA, making a total of eight. The Type IV cement i used mainly in massive structures such as dams where low heat of hydration is required. It is not normally kept in plant invento- ries, buts made for special projects as needed. For blended hydraulic cements ASTM C 595-06, Standard Specification for Blended Hydraulic Cement curently applies. ASTM C 150 ‘was originally issued as a tentative specification in 1940 and C595 in 1967. The fist ASTM specifications for cement were approved by the Society in 1904. ASTM C 1157, Standard Performance Specification for Hydraulic Cement was ‘originally approved in 1992. Federal specications generally refer to the ASTM specifica: tions, but special provisions may occasionally apply. For state highway paving projects Specification M-85 of the American Association of State Highway and Transportation Officials, (AASHTO) often applies, athough many state DOTS refer to ASTM C 150, Many individual states have their own modifi ‘ations to those specifications with which the producer must be intimately familiar For instance, some southern states in semi-tropical temperatures may have special provisions which favor concrete performance at elevated temperatures. Special limitations on cerent fineness are an example, For the northern states, durability under freezing and thawing conaitions, and resistance to de-icing chemicals may be emphasized For plants which produce cements fo ol wel driling appli cations the American Petroleum institute (AP) Specification 104 will be of primary importance. The cil field service com- panies frequently have additional proprietary requirements. ‘Many special apolications for cement call for modifications to the standard specifications. Cement used in the manufac- ture of concrete block isa common example, The manutac- turer will sometimes develop a cement for those applications which they can affer to all customers with similar needs. Occasionally individual customers require cement in sufficient Quantities to insist on their own modifications to the stan- dard specifications. The plant laboratory staff must always be familia with those requirements. An example mil tet report from ASTM C 150) shown in Figure 2.1 Sales departments are sometimes requested to submit bids ‘on cements for export which must meet foreign specitica- tions, The laboratory must determine whether thei produc- tion meets those requirements. Most are likely to be spec- fied in metric units, but the task of comparing is not as, simple as applying a corwersion factor, for in many cases the test methods are different from the standard U.S. methods, ‘The specifications ae divided into two categories: chemical requirements and physical requirements. Test methods for determining compliance wit the specications are listed in ASTM C 150 inthe section on referenced documents. The chemical tests are all included in ASTM C 114, Standard Test Methods for Chemical Analysis of Hydraulic Cement. The current designation is ASTM C 114-05, ASTM C 114 was originally published asa tentative specification in 1934. Test methods for determining compliance with the physical requirements ae sted individually inthe section of ASTM C 150 on Referenced Documents. AP! Specification 10 requires physical tests unique to oil well cements which are rot included in the ASTM test methods, ASTM test methods ray be used to show compliance with most other cement specifications curently in use in the USS. The specific standard and optional chemical parameters included in ASTM C 150 ae listed in Tables 2.1 and 2.2. ‘A shorthand notation, traditional n the industry, is used to express chemical compounds. nit S=SiQ, A=Ab03 03 C= C00 Its not unusual to find the folowing items supplementing the ist: M=MgO N=Na0 — K=K0 The standard and optional physical requirements for which thete are specication mits in ASTM C 150 are listed in Tables 2.3 and 2.4 ements of 3 Quality Cont Program ASTMC 150-05, ‘ABC Portand Cament Company ualytown, Nd ‘CamentType I Date: March 9, 1908 Production Peiod: March 2, 1908 — March 8, 1808 ‘STANDARD REQUIREMENTS ‘ASTM C 150 Tables 1 and 3 CHEMICAL PHYSICAL Spec. Test Spec. Tost tom Lit sult tem Lut Fresut 80, (%) 20min 206, ‘Aircontentof mortar (volume %) 12 max 8 0s 6) 6omax 44 Blaine fnenoss (ka) 280 min sm F203 (%) 6.0max 33 ‘Autoclave expansion () Os0max 0.08 620 (%) NA 629 ‘Compressive svength (MPa) rin M0 (%) 6.0 max 22 “aay NA 30s (%) Somx 27 Sys 70 234 gation oss (4) 3omx 27 7 days 120 208 NagO (%) NA 0.19 2a.days NA or) NA 050 “Time of setng (minutos) Insole residue (%) 75m 027 Vicat 0. (8) NA 15 Iria Notas than 45 124 LUmestone(%) 50max 35 Not more than 35 (CaCO in iestone (3) To min 8 Potential (%) 3s NA 50 cs NA a GA max 6 CyAF NA 10 uA + 2(CxA) NA 2 WA= Not applicable OPTIONAL REQUIREMENTS, ‘ASTM C 150 Tables 2 and 4 CHEMICAL PHYSICAL Spec. Test ‘Spec. Tost rn Lt Recut om Lit sult 38 + CA CH) ‘58 max 56 False sot (4) 50min w Eqvaent alkalis (9) t 052 Heat yeaton klk) See eT 7 days t 300 + Limit not spectiog by purchaser. Test result provided for Ce Information only. 28 days 20min 307 + Test result fr this producton period not yet avaiable ‘Wo cortly that the above described coment, a tho time of shipment, meets he chemical and physical requirments ofthe ASTM G 150 ~XX or (ther) speciicaton. Signature; 2t2[epeye 3 2 2 2 2 1 2 5 4 4 7 3 8 1 4 - 7 a = 1 5 2 2 0 2 3 2 1 9 1 2 8 1 6 4 2 5 7 4 4 = ] a. E} 4 1 4 7 4 4 7 2 4 1 0 2 2 5 3 3 3 7 oO 7 = 3 = = = E = 2 oO 3 2 6 2 1 z2f1[sfPs{3]«4 [2 af2},o]1}6|4 2 3 3 7 3 5 2 oO 7 = i 1 0 sf3][4¢f2{[3]}o0]5 tte fre foe ts 3 psf2f2{[3 4 ]3 @f2t3 {22 [1 ofi{[1f3 [4]ele 3.4¢t1{[2 [113 3 4 4 1 3 3 3 3 2 4 2 1 2 st3ts{[1l3/4l3 2 N=250 High = 9 low=0 ‘Average = 3.10 Std, Dev. = 1.80 Skewness = 0.643, Kurtosis = 0.319 Median = 3 54 7 x | £ | Sum |Cum.% | Tally o}is| 3] 52 1 }a9] a] 168 2 | 61 | 103 | 12 3 | 60 | 163 | 652 4 | 36 | 199 | 796 5 | 24 | 203 | e92 6 | 15 | 298 | 952 7 | 8 | 246 | 984 3 | 2| 28 | 992 9 | 2 | 250 | 1000 arable { = Frequency of occurrence ‘Sum = Cumulative sum of frequency ‘Cum. % = Cumulative frequency in percent Figure 45. Tally sheet of background radiation data, ‘The symbol is read “r factorial” and is defined asthe prod- ct ofall integers from one to . Accordingly, 3! =1-2-3=6 and 5! = 1-2-3-4:5 = 120, Zero factorial, 0! is defined in mathematics as equal to 1 In the preceding example of x-ray backoround counts, where bar = 3.10, what i the probability of exactly 6 counts being recorded in a one-second interval? P(6) = 31 (3.18/61) += 0.04505 (887.5039/720) P16) = 0.555 ‘Therefore, in a series of 250 one-second intervals, as described above, 250 (0.0555) = 13.9 or 14 in which six counts were recorded. Figure 4.5 shows that six counts were observed 15 times which is good agreement with the predic- tion ofthe Poisson distribution. The probability of zero counts would be: P(0} = e-31(3.19/01) (04505 (1/1) 4505 Ho Data Behave ~Descintve States Ina series of 250 observations, one would expect to record zer0 counts 250 (0.04505) = 11.3 or 11 times. Zero is actually observed 13 times, again good agreement with the distribution law. {An interesting feature ofthe Poisson distribution i thatthe distribution is established by a single parameter, the mean Recall that the normal distribution was established when ‘wo parameters, the mean and the standard deviation, were specified. In the Posson distribution the variance is equal to the mean. In our xray data the standard deviation is = 3.10 =176. Calculation from the square root of equa- tion 4.10 yields 1.802 which, again, is excellent agreement. At the conclusion of this tet, the background counts were accumulated for two periods of 1000 seconds each, Totals of 3062 and 3224 were obtained which isin good agreement with the average of 3.10 counts per second obtained in the ‘one-second periods. ‘The Poisson distribution is used in industrial applications when the probability of an occurrence is small, but the total ‘number of opportunities for occurrence is large. The proba- bility may be unknown, and the total number of opportuni- ties may be unknown, but a reasonable estimate of the product of the two is the mean. The number of broken bags 55 ontol of Portand Cemens Quality ina shipment of packaged cement seems a logical candidate {or application ofthe Poisson Distribution, 4.2.4, Other Distributions ‘A very large proportion of data encountered in cement plant laboratory operations may safely be considered normally dis- tributed. Some notable exceptions do occur. For instance, ‘the normal distibution contains an inherent assumption that the continuous variable can take on any value — unlimited in magnitude on the low side and unlimited in magnitude on ‘the high side. in practice there are practical limitations Consider, for example, the presence of free mein clinker intended for API Class H Cement. Attempts are made to hold it very low, but negative values cannot occur. Therefore, ero isa lower limit. On the other hand, when kilns become upset, there is a tendency forthe free lime to increase rather Table 4.6, Daily Determinatinos of Free Lime in than to decrease, During periods when the kiln operators are ‘trying to coax a coating to form across a hot spot onthe kin shell the burning criteria may be relaxed as much as possible without sacifcing overall quality of the product. The nature ‘ofthe free ime determination will lso have an effect. is ‘an extraction process with periodic titration. tis influenced by the partie size ofthe specimen and the length of time of the determination. This can resuit ina distribution skewed to the high side, Table 4.6 shows daly clinker free lime values from a single plant over a period of 18 months. Figure 46 shows the tally sheet of the frequency distribution, The tong, skewed, tail of the distribution toward the right i visual evidence of the non-normal nature, Following the same procedure as for Tobe 4.4 Tale 4.7 is constructed and the non-normal nature is shown via the 2 test. The average 180.419 and the standard deviation is 0.156. jinker Production ata Single Plant ‘The input data are 044 ] 034 | 029 | 043 | 040 | 047 | 056 | 038 | O47 | 054 | 048 | 040 o47 | 039 | 034 | 043 | 040 | 036 | 038 | 037 | o42z | o40 | 038 | 037 039 | 035 | osz | o42 | 044 | 059 | 062 | 068 | 075 | 057 | 074 | 072 074 | 047 | 057 | 066 | 060 | 039 | 034 | 033 | 023 | 021 | 035 | 027 048 | 051 | 036 | 035 | 035 | 035 | a54 | 021 | 030 | 023 | 0.26 | 031 027 | 032 | 030 | 085 | 065 | 068 | 050 | 064 | 056 | 046 | 04s | 043 054 | 042 | 042 | 046 | o42 | 062 | 033 | 015 | 033 | 035 | 054 | o5s 040 | 032 | 075 | 069 | 066 | 053 | o45 | os4 | 045 | o67 | 057 | o42 04s | 034 | 033 | 034 | 045 | 034 | 025 | 026 | 026 | 026 | 020 | 020 023 | 037 | 030 | 025 | 020 | 015 | 050 | 027 | 026 | 026 | 021 | 020 023 | 022 | 017 | 019 | 029 | 028 | 031 | 028 | oa | 028 | 0.20 | 025, 032 | 031 | o41 | 039 | 038 | 038 | 040 | 044 | 034 | 036 | 030 | 019 035 | 039 | 027 | 034 | 030 | 045 | 030 | 044 | 060 | 073 | 061 | o59 035 | oso | 044 | 043 | 035 | 026 | 026 | 018 | 017 | 043 | 047 | 040 os7 | os | 055 | 027 | o42z | 072 | 035 | 026 | 0.26 | 038 | 069 | 078 032 | 032 | o48 | 037 | o44 | 032 | 048 | 038 | 040 | 049 | 0.39 | 045 043 | o40 | 049 | 045 | 0.26 | 031 | 052 | o40 | 034 | 022 | 036 | 033 023 | 026 | 031 | 038 | 027 | 015 | 052 | 039 | 026 | 026 | 026 | 033 020 | 040 | 053 | 032 | 046 | 057 | 058 | 086 | 088 | 060 | 050 | 070 oso | 078 | 058 | 043 | 054 | 038 | 055 | 037 | 040 | 070 | 0.46 | 035 os3 | 079 | oss | 076 | 095 N=265 High = 0.95 Low = 0.15 ‘Average = 0.419 St. dev. = 0.156 Skewness = 0.768 Kurtoss = 0.343 Median = 0.4 { f Class Interval 0.144 to 0.194 0.194 to 0.244 0.244 to 0.294 0.294 to 0.344 0.344 to 0.394 0.394 to 0.444 0.444 to 0.494 0.494 to 0.544 0.544 to 0.594 0.594 to 0.644 0.644 to 0.694 0.694 to 0.744 0.744 to 0.794 0.794 to 0.844 0.844 to 0.894 0.894 to 0.944 0.944 to 0.994 f | Sum BRoe 122 187 22 | 179 18 | 197 15 | 212 8 7 28 33 | 86 36 35 ‘Cum, % | Tally Figure 46. Grouped frequency distribution. Table 4.7. Tes for Goodness of Fit of Free Lime Data to a Normal Distribution 33 102 216 354 498 64 BA 804 865 898 93.4 959 98.4 98.4 996 998 100.0 How Daa Behave - Descpive Satis a ° Area of E (one? Class interval__| Observed frequency | _normal curve __| Expected frequency 3 0 0.0396 96 9.600 0.144 0.194 8 0.0356 87 0.056 0.194 0.244 7 0.0564 38 0.742 0.244 -0.294 2B 0.0805 197 3.497 0.294 -0.344 33 0.1038 25.4 2274 0.344 -0.394 36 0.1210 297 1.384 0.394 -0.444 35 0.1274 312 0.463 0.444 ~ 0.494 2 0.1210 297 1.951 0.494 - 0.544 18 0.1038 25.4 2.156 0.544 - 0.594 15 0.0805 19.7 1.121 0.594 - 0.644 8 0.0564 138 2.438 0.644 - 0.694 8 0.0356 ar 0.056 7 0.0390 96 5.704 E=245 17.0000 2448 31.442, 37 Convo of Porton Cement Quatty Note that in Table 4.7 the numberof cells ae reduced to 13 to accommodate the restrictions previously explained with regard to the minimum expected frequency of five per cell The number of degrees of freedom is obtained by sub- ‘acting one forthe total number of observations (245), an additional one forthe average, and one forthe standard de- viation, both of which were calculated from the same sample ‘of data, The degrees of freedom, therefore, is 13 ~3 = 10. From the tables of the 32 probabilities, for 10 degrees of freedom, the probability of obtaining a value of 72 as large 5 31.442 is less than 0.001 or 0.1%. Itis concluded at the ‘90% confidence level thatthe dstibution of fee lime at this plants not Gaussian over an extended period of 18 months. ‘A more detailed examination ofthese data and some further analysis of the data may lead to a better understanding of the distribution and what action may be helpful. Asymmetrical distributions are not unusual. They do not imply lack of control. Had the chi-square test for goodness of fit alowed us to conclude that the sample of data was from a normal, or Gaussian distribution, however, it would ‘ot have implied thatthe process was under control, for demonstration that a distrbution is normal isnot a sufficient condition of contro. Consider quantitative measures ofthe distortion of asym metrical distributions. There are two characteristics to be considered. Ifthe cistibution i lopsided with one side ‘extending father from the mean than the other its said to be skewed toward the long tai: positively skewed if the long tail isto the right as in Figure 4.6; negatively skewed ifthe long tai isto the lft. A symmetrical distribution has a coeff cient of skewness of zero. However, a valve of g1=0 does not prove or even imply that a distribution i symmetrical or normal. simply does not lead to rejection of the normal typothess. The most common measure of skewness is: 1n-= number of observations = root mean square deviation (standard deviation) i= individual value ofthe variable = variable (the mean of the variable). The value of gy may be either postive or negative. ‘The other characteristic to be described isthe kurtosis. The ‘word is from the Greek word for convexity and refers to how the values are distributed near the middle of the frequency 58 distribution. If the variable tends to be more concentrated ‘than normal near the mean, the distribution tends to be “peaked” and the kurtosis is positive. If the central portion is more spread out than normal and tends to be somewhat, fiat, the kurtosis is negative, The coefficient of kurtosis is defined to be equal to 2210 for a distribution near normal, but a coefficient of zero does not prove or imply normality. The quantitative measure is as follows: 6.18) 9-2 where: 92 = coefficient of kurtosis n= number of observations ‘6 = root mean square deviation (standard deviation) +x|= individual value ofthe variable variable (xis the mean of the variable) ‘The value of gp may be either positive or negative ‘The symbolism for skewness and kurtosis not uniform in the literature. For this example, the practice of The Manual ‘on Presentation of Data and Control Chart Analysis (ASTM £2000, pages 19-20) was followed with an exception: the symbol forthe population standard deviation is used above ‘to designate the root mean square deviation (standard dev- ation) of the sample as though the sample were a finite population, Note of course that the fourth power of the standard deviation is the square of the variance ‘Shewhart discussed the skewness and kurtosis and used the Coefficient of skewness as defined above along with the ‘normal distribution to fit asymmetrical distributions to test data. He referred to the combination as a “second approxi- mation” (Shewhart 1931, pages 89-98). The ASTM Manual (mentioned above) discusses the subject and gives tables of factors which can hep fit asymmetrical distributions to test data (ASTM 2002, pages 19-29). Duncan discusses skewness ‘and kurtosis on pages 64 and 584-589, He suggests how the coefficients of skewness and kurtosis may be used to test for normality of a distribution and gives tables with the 0.95 and (0.99 0.05 and 0.01) probability points ofthe sampling deviation rather than as the ‘sample deviation, s. In a normal Me distribution that probability is 0.0026 (0.26%). So there are © jimits on what we can expect even from some very unusual destributions of data. ( When describing distributions of laboratory data always ‘eport the number of determinations, the arithmetic mean, ee the sample standard deviation. That information alone => coniveys the essential information for a majority of the uses nae ofthe data. the uber of obsevatns ge {ebout 250 or more) the coefficient of skewness should be | pserted along wih a grouped tequeny dstrbtonn the form of a histogram. © The range of values in small samples of data provides a © simple relationship with which to obtain an unbiased estimate cof the population standard deviation from wich the samples ‘came. It can be applied to data from duplicate test to esti mate the singleab precision forthe determination. ..-A sight variation on the use of the range may be applied to paired samples to estimate single-ab precision pooled over all the labs participating inthe test. A comparison of the pooled single lab precision to the muita precsion on the ~ same samples may aid in detecting the existence of labora- tory bias in the specific test procedure. Graphical techniques = canassist in the effort. ‘The moving range of two consecutive determinations during = production provides an estimate of the standard deviation of a process without the influence of major long-term cycles in ~ the process average. This technique willbe useful in devel- oping quality contro charts, How Data Behave Desc Statis 67 Statistics formulas are used to understand the distribution of sample means and they provide critical information for hypothesis testing. F — 5 HOW DATA BEHAVE — INFERENCE AND PREDICTION escriptive statistics provides a means of examining a sample of data from a population and calculating ‘well-defined and readily understood mathematical parameters. Those parameters, in turn, allow others ‘who may have use of the data to reconstruct the distribution of the data in most ofits important charac- teristics. The parameters recommended for that purpose consist of: (1) the arithmetic mean as a measure of central tendent (2) the variance, or the standard deviation which is the square root of the variance, as a measure of dispersion of the data; (3) the coefficient of skewness as a measure of the lopsidedness of the distribution (neg- ative skewness toward the left and positive skewness to the right); and (4) the coefficient of kurtosis to describe any tendency toward flatness (negative kurtosis) or peakedness (positive kurtosis). The skewness and kurtosis are increasingly important when larger samples of data are examined - approaching ‘The parameters referred to above are sample parameters ~ the sample mean, the sample standard deviation, the sample skewness, etc. A better knowledge of the population mean, the population standard deviation, the population skewness, etc. is preferred. Those parameters of great importance generally will remain unknown in a vry large population or in an infinite population Methods of statistical inference provide procedures by which ‘one can generalize from the information obtained from the sample to the information needed about the population. Examples of inference are seen so frequently, sometimes they are taken for granted. For instance, this yer, 2006, is an election year for many high poitical offices: all members of the US. House of Representatives, one-third of the members of the US. Senate, and many state and local officials. People will be bombarded with results of pols - samples of public opinion from perhaps a few thousand voting citizens. Meth- os of inference allow the posters to extrapolate from their Palls to generalizations about what the desies of the voting Population, numbering in the mult-milions, might be and how they might vote if the election had been held con- Currently withthe poll. Thankful, this problem ~ devoid of human idiosyncrasies —is alittle easier, but many of the 50 and beyond. techniques will progress along simiar approaches. A litle ‘mot information about the distribution of sample means will help. 5.1. Distribution of Sample Means tn Chapter 4, a sample of Wagner fineness data was examined, and evidence was developed which supported a conclusion that the data were from a normal distribution ‘A sample of data on fee ime in clinker was ako examined, and the evidence was developed which led toa conclusion that the data were not from a normal distribution. Examina- tion of the conditions under which the clinker was produced, and the quality guidelines accepted atthe time, shed some light on the possibilty thatthe distribution may be the sum of two separate normal distributions wth different means and standard deviations resuiting from different burning conditions. Consier the two cases below. 5.1.1, Sampling From a Normal Distribution {population is normally distributed with a mean y, and standard deviation , then the mean (x-bar) calculated from random samples of size n taken from the population wil also possess a normal distribution with mean y, and variance of 69 Contra ofPrtand Cement Quay .o2/n, The distribution of many x-bars collected in accordance ‘with this staterent is generally referred to asthe sampling distribution of the mean. inthis case its the means of random samples from @ normal population. Note that two different distributions are being compared. One is the popu- lation of individual values. The other isthe population made Up of the means of all possible samples ofthe given size from the universe of individual values. The means of both Populations are equa toy. The variance of the population of individual values is c2- And the variance ofthe population cof sample means (s-bar is 62/n, The standard deviation of the x-bar values, therefore, i: ox=0Wn Consider how this applies to daily quality contol. in the control ofthe lime factor or the lime saturation factor, slica ratio, and AVF ratio atthe raw mil discharge its likely that samples of the discharge are taken for chemical analysis and perhaps a determination ofthe amount retained onthe No. 325 sieve on an hourly basis. In a wet process plant the percent water in the slurry would be determined. A portion of each sample would be retained, Action to control each para- meter around a fixed holding point (mean value) would be taken as necessary. Under these conditions the distribution ofthe value ofthe control parameter could be expected to approach a normal distribution. At the end of each shift the range of the eight determinations may be calculated and the mean may be calculated. The standard deviation of the eight individual values may aso be calculated. At the end of each day equal portions ofthe 24 periodic samples may be com- bined into a single sample and mixed wel. Determinations may be made on this single sample to represent the day’ production. While a single determination on a single sample is given, the statistical theory gives added confidence that the sample is from a normal distribution and thatthe dstib- ution ofthe daily test results will be normal. But suppose the population of individual values deviate from a normal cistib- tution; what can be expected? (6.1) 5.1.2. Sampling From a Non-normal Distribution If x possesses a distribution witha finite mean p, and afrite variance of 6, then the sample mean, x-bar, based on a sample of size n, will have a distribution which approaches 2 normal distibution wth mean p, and variance o2/n sn increases The distribution of the individual values, therefore, may be either normal or non-normal. The only restriction is that the 70 mean and the variance be finite. But how much does n have to increase? In theory the distribution ofthe means reach that of a normal distribution when n becomes infinite. That may not be of great value. But in practice it can be seen that the distrbution of the means start to approach that of a normal distribution at moderately low values of n even when the distribution ofthe individual values deviate markedly from the normal. individual values deviate onty sightly ‘rom the normal, then the means of samples of even low Values of n will tend toward the normal distribution. Values of nas low as n= 4 will have only one half the variability about the mean ofa near-normal distribution that the indi- \idual valves have. Even in the most severe cases samples composed of n = 25 will noticeably tend toward normal Note that these theories are not limited to continuous variables: they also apply to discrete variables ‘The statistical principle stated above for non-normal popula- tions is commoniy referred to as the central limit theorem. & roof of ether of these principles is beyond the scope of this text. Discussions of both may be found in Hoel (Hoel 1932, pages 120-132) and in Dixon and Massey (Dixon 1969, pages 43-50 and 58-61). Duncan offers discussions and proofs (Duncan 1974, pages 124-139 and 903-904). 5.1.3. Confidence Limits for Means The discussion of the normal distribution included use of the area under the normal curve as a means of estimating the number of occurences to expect within given ranges, Those applications presuppose a knowiedge ofthe population mean and the population standard deviation, or an assumption concerning those parameters. In. most cases the total information on a problem slimited to what can be extracted from a sample of data. One must rely (onthe sample mean, x-bar, as an estimate ofthe population mean and the sample standard deviation, s, as an estimate of the population standard deviation, WS. Gossett studied the relationship between the popula tion mean and thee items: (1 the sample mean, (2) the sample standard deviation, and (3) the number of ites in a sample. He expressed the relationship mathematically in the variable, t, which he developed: The distribution of the variable is known as "Student t distribution.” ‘The variable t can be understood more easily by comparing it to the standard normal variate, 2 = (~ 1), and realing that it refers to individual values of x. Replace the individual value of x with x-bar, the sample mean, and replace the population standard deviation with the standard deviation of ~ the sample mean as defined by the central mit theorem, quate that to t and Student's variable is given. 62) t= EBs With thet variable, work with problems involving the popu- {ation mean, p, when the population standard deviation is unknown. The t distribution is symmetical but itis not Gaussian, It depends on the value of n. AS n increases, t becomes closer to the variable 2 and its distribution is the same as the normal distribution when n becomes infinite © Tables ofthe t distribution are available in most technical handbooks. A limited table of the t distribution is provided in ‘able 24. It gives critical valves of the variable t corresponding ‘to various probabilities and the number of degrees of free- dom. In this case, the degree of freedom is one less than n; v=n-1, The value of p at the top of each column gives the probability that the calculated value of t will exceed the value Of t listed in that column if the sample is from a normally distributed population. Since the distribution is symmetrical, it also gives the probability that t will lie to the left of the ‘corresponding -t value. For instance, with a sample size of 1n=8, the degrees of freedom are 8~1 = 7. Entering Table ‘2A under column heading p = 0.025 and going down to the line v =7 find that there is a 0.025 probability of t exceeding 12.365 and a probability of 0.025 of t being less than -2.365. ‘Therefore, there is a 95% confidence level (p = 0.95) that t lies between -2.365 and +2.365. The mathematical statement i: P(Itl $2.365)=0.95 forn=8 or: P({tl > 2.365)= 0.05 forn=8. ‘These are read: “The probability that the absolute value of 1 is less than or equal to 2.365 is equal to 0.95," or “The probability thatthe absolute value of tis greater than 2.365 is equal to 0.05." If Pis the confidence level, the probability of exceeding Pis 1-P =o. Since the distribution is symmet- ical, «is divided equally between the far right tal ofthe curve and the fr lft tail ofthe curve with a/2 on each side. Write that as: “tan tare and (@—pWn/s< tara How Data Sehae~nfrence and Picton Since both s and Jf are positive quantities, both sides of ‘each inequality can be multiplied by s//f and rewritten: H-p> tan) shin and Xp < (tara) SAMA Rearranging once more to place the population mean, pon the positive side of each inequality it becomes: + (taa)sMYn >y and X- (tan)sin< 4 ‘which states thatthe population mean, p, can be expected to lie between a maximum of x +(taia)s/n and a mini- mum of x ~(taa)s/Yn. This s equivalent to: 63) %-(tendsncp 20.0%. f shown cause to reject the hypothess that p = 20.0% or any value less than 20.0%, one will accept the alternate hypothesis that the true value of Si, is greater than 20.0% and thus meets the specification on SiO 2. Choose a level of significance. This requies that one ‘agrees on the level of risk to take of passing a production cr shipment which actually fails to meet the specification. ‘nother words, what probability that a true hypothesis will be rejected ae they wing to accept? Ths type of ero is referred to as an alpha error. In this case if they reject the hypothesis when i s actually true, they may have the ship- iment rejected later by a customer for not meeting the spectcation. A beta error could lead, unnecessarily, to blend the cement back into the system or market it where those Type I specifications do not apply. ‘Assume that they will accept the true hypothesis 95% of the time (P = 0.95, (1-P) = 0.05) ow Data Behave Inference and Pedic 3. Select a probability distrbution. The Central Limit ‘Theorem leads one to assume the mean of the test results, will tend toward a normal distribution 4. Choose a region of rejection. ths problem, only high values will ead to rejection of the hypothesis. Therefore, be concerned only withthe right sie of the normal distr- bution cum. Thisis frequently called a “single-tlled test." Look for a limit having 0.05, or 5%, of the area stil to the right and 9596 to the left. From Table 1 the value ‘of 2 for which 5% ofthe determinations is greater than 2 is found to be 1.645, Therefore, assuming the true value (of SiO isu = 20.0 s the population mean, reject the hypothesis, Hp: w$ 20.0 if zis greater than 1.645 and accept the alternate hypothesis that Hy: p> 200. 5. Perform the calculations. From the test data it is known f= Zand x= 20.16, The standard deviation of the SiO determination is needed. From laboratory test programs ‘one know this to be very dose to 6 = 0.13. Keep in mind that they would expect another lb to test a specimen from the same sample. Using equation 4.13 for the average of two determinations: (= u)/0)vn (20.16 -20.0)/0.13)\2 2174 6. Make the mathematical decision. Since the value of zis in the rejection zone there is evidence at the P= 0.95, (1 =P) = 0105, level that the true value of iQ is not less than 20.0%. Reject the original hypothesis and accept the alternate. 7. Make the supervisory decision. At this point, the judge rent factors come into play if confident ofthe valiity ofthe standard deviation (a = 0.13) and the test results, then release the cement for shipment or further test a Type cement, expecting another lab to agree with us about 95% of the time, Note, however, that if the popu lation standard deviation is greater than 0.14 and this test is applied then accept the hypothesis. Furthermore, if one is only wiling to accept a risk of 1% of rejecting a true hypothesis, the critical value of z would be 2 = 2.327, and the hypothesis would have been accepted. If non- mathematical factors must be considered, and they are Persuasive onthe side of caution, then it might be appro- priate to resample and retest, adding the new data to the ld data ‘As an example, the citical value of z fora probability of P= 0.99, (1 ~P) = 0.01, is 2.326. Ifthe average SiOz of 5 onto Poctand Cement Quay 20.1696 is an average of four determinations rather than ‘two, then the calculated zis z= 2.462, and the hypothesis ‘would be rejected with 99% confidence and the alternate accepted. The supervisory decision lies outside the arena of data analysis ts indicated here asa step inthe hypothesis testing to show that one ofthe purposes of data analysis is to contribute information forthe benefit of management. While its a valuable aid to judgment; itis not a substitute {or judgment. A marginal situation has been outined in which a supenisory decision must be made. Note that it did ‘ot prove the cement met the specification. That cannot be done with the data avilable The sample of hypothesis testing expanded on above i typical of the general case of drawing inferences about a mean when the population variance is known. When the population variance is unknown, more test data would be needed and the student t test would be used with the estimate ofthe variance (52) determined from the data. For further information on that specific test see Hoel 1971, pages 170-171; Bryant 1966, pages 84-87; and Diron 1969. A study of these references wil confirm the qualitative con- clusion that any time while working within three standard deviations of a specification limit, one can expect trouble ‘on occasion and alot of extra testing 5.2.3. Inferences about Variances There are many occasions to seek information about vara- bilty ofa control parameter or a test procedure. Fr instance, ‘a question in Chapter 4 was noted along these lines: if a standard deviation on the Wagner fineness of 7.5 mé/kg is found for a 25-day period of production versus 5.0 m2/kg forthe previous 25-day period, can one tell whether this represents a change in uniformity ofthe product or merely reflects a normal variance of the standard deviation? if one ‘wanted to show whether an innovative process change had resulted in an improvement in uniformity of a qualty charac- teristic would they know how to make a quantitative com- parison? This could be represented by an experimental roup and a control group produced under essentially the same contitions. For instance, they might compare a period of production with no grinding aid and one in which a ainding aid was used, or compare two periods of production with two different grinding aids, These questions can be set up as a test of the hypothesis that the variances of the two popu lations are equal. To do so introduces a new frequency distribution usualy called the “F distribution.” it was ‘originally discovered by Sir Ronald Fisher in asightly 76 different frm, but GW. Snedecor modified and simplified the values, and named itn honor of Fisher (Volk 1969, age 159). ts mathematical form is simply (6.4) F 28? (xg) /5? 04) where s? (x9) and s2 6) are the sample variances ofthe two variables, xp and x, which have been determined from ny and ay measurements respectively. The F ratio of variances from normal populations has been. studied, and the frequency distribution has been derived ‘mathematically and tabulated for easy application. f the two variances do infact representa single population or universe (ie, the two population variances are equal, then the ratio depends on the degres of freedom of the two samples, which may be diferent: vp = np 1, and vy = 9) — 1. ‘would be possible to approximate an F distribution experi= mentally. Suppose many samples (perhaps as many as 100,000) were taken of ten items each from a population just as Tables 5.1 and 5.3 were formed, and many samples, of five items each were taken similarly. The variances of each sample could be calculated and a ratio formed by selecting pairs at random with the variances of the sample often always in the numerator and the variance of the samples of five in the denominator. The value of the ratios would vary from near zero to large numbers, but the average value ‘would be near unity and the distribution would be skewed strongly to the right toward the high values. if they were grouped in a frequency distribution similar to Figure 47 it would be found that 95% of the values would be less than 6.00, and 99% would be less than, 14.66 Ifthe ratios were reversed and the variances ofthe samples of five are placed in the numerator and the samples often in the denominator then it will be found that 95% ofthe values wil be less than 3.63 and 99% wil be less than 6.42, So certain are these {quantities that i value of F exceeds them it can be assumed with the indicated degree of confidence that one ofthe vari ‘ances didnot come from the same population asthe other. Therefore, the F rato of variances can be used asa test of the hypothesis thatthe two variances are equal, if agreed to place the larger variance in the numerator then use the Upper end of the tables (high values) only, Table A3 covers the 95% level (P = 0.95; (1 ~P) = 0.05) and the 99% level (P=0.99;(1 -P)= 0.01) which afrequently used for this ‘purpose, Note thatthe two samples used to form the ratio. ate no required to have equal means. Table 34 isan example of the manner in which the F dis- tribution is tabulated. The table must be entered with the degrees of freedom for the numerator across the top, and the deorees of freedom for the denominator down the left side. More extensive tabulations may be found in Perry 1984, pages 1-25; Beyer 1981, pages 549-554; Duncan 1974, pages 959-964; Hoel 1971, pages 292-295; Dixon 1969, pages 470-485; Bryant 1966, pages 310-313; and Volk 1969, pages 406-409 The steps in the hypothesis test previously outlined can be followed. 1. State the hypothesis and the alternate. inthis case, state the hypothesis that Hp 012 = 0. If one cannot find evidence that this is tre, simply accept the alternate that they are not equal and the variance in the numerator is the larger: Hy: 02 > 072, 2. Choose a level of significance. Choose P = 0.95 whichis an arbitrary choice. (Ii simply for seeking information: 3. Selecta probability distribution. The two samples of data ‘were selected in such a way that the Central Limit Theorem leads one to believe that both samples represent a normal Population. Therefore, the F distribution described above is appropriate for this problem, 4, Choose a region of rejection. Only very high values of F will ead to rejection of the hypothesis since it was agreed ‘0 place the larger variance in the numerator. The region of rejection i found from Table A3 using the P = 0.95, (1-P) =0.05, portion ofthe chart. There are 25 determi- nations in each estimate of s®so we enter the 5% chart with 25 — 1 = 24 degrees of freedom for the numerator and 24 deorees of freedom for the denominator. The crit- ical value of Fis F = 1.98, and the region of rejection is any F greater than this value 5. Calculate F from the test data, F=752/5.02=225 6, Make the mathematical decision, Reject the hypothesis thatthe two variances are equal and accept the alternate that there has been @ changin te variance resulting in less uniform fineness in the recent period 7. Make the supervisory decision, The variance test gives no information on cause and effect. The supervisory decision must be based simply on the knowledge thatthe fineness cof recent production was more variable than previous pro duction. A reasonable course would be to seek informa tion to differentiate between whether the increase in \arabilty resulted from increased variance of the test procedure or increased variance of the fineness from the process. The frst could result from less stable equipment andor chemicals used or from different operators with Ho Ota Behave — Inference and Prediction

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