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Introduction to Statistically Designed Experiments

Statistically designed experiments can save researchers time and money by reducing the number of necessary experimental trials, while resulting in more conclusive experimental results. Surprisingly, many researchers are still not aware of this efficient and effective experimental methodology. As reported in a 2013 article from Chemical & Engineering News, there has been a resurgence of this methodology in recent years (http://cen.acs.org/articles/91/i13/Design-Experiments-Makes-Comeback.html?h=2027056365). This presentation will provide a brief introduction to statistically designed experiments. The main advantages will be reviewed along with the some basic concepts such as factorial and fractional factorial designs. The recommended sequential approach to experiments will be introduced and finally a case study will be presented to demonstrate this methodology.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

The application of statistically designed experiments to resistance spot welding

State-of-the-art Resistance Spot Welding (RSW) equipment has the potential to permit realtime monitoring of operations through advances in computerized process control. In order to realize adaptive feedback capabilities, it is necessary to establish correlations among process variables, welder outputs, and weldment properties. The initial step toward achieving this goal must involve assessment of the effect of specific process inputs and the interactions among these variables on spot weld characteristics. This investigation evaluated these effects through the application of a statistically designed experiment to the RSW process. A half-factorial, Taguchi L sub 16 design was used to understand and refine a RSW schedule developed for welding dissimilar aluminum-lithium alloys of different thickness. The baseline schedule had been established previously by traditional trial and error methods based on engineering judgment and one-factor-at-a-time studies. A hierarchy of inputs with respect to each other was established, and the significance of these inputs with respect to experimental noise was determined. Useful insight was gained into the effect of interactions among process variables, particularly with respect to weldment defects. The effects of equipment related changes associated with disassembly and recalibration were also identified. In spite of an apparent decrease in equipment performance, a significant improvement in the maximum strength for defect-free welds compared to the baseline schedule was achieved.

Hafley, Robert A.↗

The effects of Cr, Co, Al, Mo and Ta on the cyclic oxidation behavior of a prototype cast Ni-base superalloy based on a 2(5) composite statistically designed experiment

A series of cast Ni-base superalloys were systematically varied at selected levels of Co, Cr, Mo, Ta, and Al. The elemental levels varied were Mo, 0 to 4 percent; Cr, 6 to 18 percent; Co, 0 to 20 percent, Ta, 0 to 8 percent; and Al, 3.25 to 6.25 percent. The cyclic oxidation resistance was determined from specific weight change data as a function of time for 1 hr cycles in static air at 1100 C. The significant terms in decreasing order of their importance were Al, Ta, Cr2, Al-Cr, Cr-Co, Co2, Al-Mo, Cr-Mo, Al-Al, and Mo-Ta. The Al term alone accounted for close to 82 percent of the explained variability. The estimating equation showed that the Al level was the most important and should be at its 6.25 wt % maximum value. The Mo and Ta levels should also be at their maximum 4 and 8 wt % respectively. The cobalt composition should be as low as possible, i.e., 0 wt%. The Cr level optimum varies depending on the other 4 levels. The X-ray diffaction results indicate the most protective scales are alumina/aluminate spinel stabilizized with a tri-rutile oxide high in Ta and Mo.

Barrett, C. A.↗

SSSFD manipulator engineering using statistical experiment design techniques

The Satellite Servicer System Flight Demonstration (SSSFD) program is a series of Shuttle flights designed to verify major on-orbit satellite servicing capabilities, such as rendezvous and docking of free flyers, Orbital Replacement Unit (ORU) exchange, and fluid transfer. A major part of this system is the manipulator system that will perform the ORU exchange. The manipulator must possess adequate toolplate dexterity to maneuver a variety of EVA-type tools into position to interface with ORU fasteners, connectors, latches, and handles on the satellite, and to move workpieces and ORUs through 6 degree of freedom (dof) space from the Target Vehicle (TV) to the Support Module (SM) and back. Two cost efficient tools were combined to perform a study of robot manipulator design parameters. These tools are graphical computer simulations and Taguchi Design of Experiment methods. Using a graphics platform, an off-the-shelf robot simulation software package, and an experiment designed with Taguchi's approach, the sensitivities of various manipulator kinematic design parameters to performance characteristics are determined with minimal cost.

Barnes, John↗

Case Studies for the Statistical Design of Experiments Applied to Powered Rotor Wind Tunnel Tests

The application of statistical Design of Experiments (DOE) to helicopter wind tunnel testing was explored during two powered rotor wind tunnel entries during the summers of 2012 and 2013. These tests were performed jointly by the U.S. Army Aviation Development Directorate Joint Research Program Office and NASA Rotary Wing Project Office, currently the Revolutionary Vertical Lift Project, at NASA Langley Research Center located in Hampton, Virginia. Both entries were conducted in the 14- by 22-Foot Subsonic Tunnel with a small portion of the overall tests devoted to developing case studies of the DOE approach as it applies to powered rotor testing. A 16-47 times reduction in the number of data points required was estimated by comparing the DOE approach to conventional testing methods. The average error for the DOE surface response model for the OH-58F test was 0.95 percent and 4.06 percent for drag and download, respectively. The DOE surface response model of the Active Flow Control test captured the drag within 4.1 percent of measured data. The operational differences between the two testing approaches are identified, but did not prevent the safe operation of the powered rotor model throughout the DOE test matrices.

Overmeyer, Austin D.↗

Statistical detection of differentially abundant ions in mass spectrometry-based imaging experiments with complex designs

Mass Spectrometry Imaging (MSI) characterizes changes in chemical composition between regions of biological samples such as tissues. This translates into a statistical goal of class comparison, i.e. determining analytes that change in abundance between conditions more systematically than as expected by random variation. To reach accurate and reproducible conclusions, statistical analysis must appropriately reflect the initial research question, the design of the MSI experiment, and all the associated sources of variation. This manuscript highlights the importance of following these general statistical principles. Using the example of two case studies with complex experimental designs, and with dierent strategies of data acquisition, we demonstrate the extent to which choices made at key points of this workflow impact the results, and provide suggestions for appropriate design and analysis of MSI experiments that aim at detecting dierentially abundant analytes.

NanoDESI, mass spectrometry, MSIQuickView↗

Statistical Design of Experiments Enables Rapid Exploration of Perfluorobutane Sulfonate Degradation

The phase-out of long-chain PFAS has led to the proliferation of highly recalcitrant short-chain analogs, and mineralization technologies for these short-chain PFAS are needed to mitigate their deleterious effects on environmental and human health. In this study, we utilize a statistical design of experiments, specifically, response surface methodology, to rapidly evaluate the electrochemical degradation of the short-chain PFAS, perfluorobutane sulfonate (PFBS). We evaluate the impacts of the three primary electrochemical parameters (concentration of PFBS, concentration of supporting electrolyte, and applied current) over multiple orders of magnitude on the three primary reaction outcomes of electrochemical PFBS degradation (incomplete PFBS decomposition, complete PFBS mineralization as fluorine, and anodic energy consumption). Our results correspond with literature and clearly identify the well-known tradeoff between energy consumption and complete mineralization. Intriguingly, partial PFBS decomposition and energy consumption demonstrate nonlinear dependencies in the current/supporting electrolyte concentration space and the current/PFBS concentration space, respectively. These findings highlight the utility of the response surface methodology model to efficiently interrogate a large parameter space, identifying both common results and less-obvious interactions between electrochemical parameters and their influences on reaction outcomes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Understanding and improving anode performance in an alkaline membrane electrolyzer using statistical design of experiments

The behavior of the oxygen-evolving positive electrode (i.e. anode) in the anion exchange membrane water electrolyzer (AEMEL) is complex and influenced by several factors. Very few studies have been performed to understand oxygen evolution reaction (OER) behavior by optimizing the individual factors that influence performance. Here, this study highlights the effects of catalyst loading, catalyst selection, porous transport layer (PTL) type and conductive additive content. The influence of each factor is elucidated through a design of experiments (DoE) approach with a full statistical analysis. Electrochemical data, alongside Pareto charts, parametric trends and their mutual interactions are discussed. This DoE approach is also helpful in making useful predictions and discovering new combinations to be tested. The end result was a high-performance AEMEL able to operate at a current density of 1.0 A/cm 2 at 1.80 V with IrOx OER and PtNi hydrogen evolution reaction (HER) catalysts using 0.3 M KOH fed to the anode. Even lower operating voltage was observed with PbRuOx catalyst at the anode, 1.64 V @ 1.0 A/cm 2 , though the cell decay rate was higher. Lastly, a IrOx/PtNi cell was stably operated continuously for 30 days (720 h) at 1.0 A/cm 2 . This study can serve as a guide for optimal electrode design with insights into component-performance compromises, which can aid in making design choices and performing techno-economic analyses.

08 HYDROGEN↗

Experiences in the Practice of Design of Experiments at NASA

Statistical design of experiments (DOE) has gained recognition within NASA by spurring innovation and efficiency, and it has demonstrated significant impact. Aerospace research and development benefits DOE techniques by accelerating learning, maximizing knowledge, ensuring strategic resource investment, and informing data-driven decisions. In practice, DOE relies on multidisciplinary collaboration to develop solution strategies that integrate statistical methods with subject-matter expertise to meet challenging research objectives. This presentation shares experiences in the practice of design of experiments at NASA in aeronautics, space exploration, and atmospheric science.

Peter A. Parker↗

Development of superalloys by powder metallurgy for use at 1000 - 1400 F

Consolidated powders of four nickel-base superalloys were studied for potential application as compressor and turbine discs in jet engines. All of the alloys were based on the Rene' 95 chemistry. Three of these had variations in carbon and A12O3 contents, and the fourth alloy was chemically modified to a higher volume fraction. The A12O3 was added by preoxidation of the powders prior to extrusion. Various levels of four experimental factors (1) alloy composition, (2) grain size, (3) thermomechanical processing, and (4) room temperature deformation plus final age were evaluated by tensile and stress rupture testing at 1200 F. Various levels of the four factors were assumed in order to construct the statistically-designed experiment, but the actual levels investigated were established in preliminary studies that preceded the statistical process development study.

Calhoun, C. D.↗

A designed experiment in stitched/RTM composites

The damage tolerance of composite laminates can be significantly improved by the addition of through-the-thickness fibrous reinforcement such as stitching. However, there are numerous stitching parameters which can be independently varied, and their separate and combined effects on mechanical properties need to be determined. A statistically designed experiment (a 2(sup 5-1) fractional factorial, also known as a Taguchi L16 test matrix) used to evaluate five important parameters is described. The effects and interactions of stitch thread material, stitch thread strength, stitch row spacing and stitch pitch are examined for both thick (48 ply) and thin (16 ply) carbon/epoxy (AS4/E905L) composites. Tension, compression and compression after impact tests are described. Preliminary results of completed tension testing are discussed. Larger threads decreased tensile strength. Panel thickness was found not to be an important stitching parameter for tensile properties. Tensile modulus was unaffected by stitching.

Dickinson, Larry C.↗

Maximizing Macromolecule Crystal Size for Neutron Diffraction Experiments

A challenge in neutron diffraction experiments is growing large (greater than 1 cu mm) macromolecule crystals. In taking up this challenge we have used statistical experiment design techniques to quickly identify crystallization conditions under which the largest crystals grow. These techniques provide the maximum information for minimal experimental effort, allowing optimal screening of crystallization variables in a simple experimental matrix, using the minimum amount of sample. Analysis of the results quickly tells the investigator what conditions are the most important for the crystallization. These can then be used to maximize the crystallization results in terms of reducing crystal numbers and providing large crystals of suitable habit. We have used these techniques to grow large crystals of Glucose isomerase. Glucose isomerase is an industrial enzyme used extensively in the food industry for the conversion of glucose to fructose. The aim of this study is the elucidation of the enzymatic mechanism at the molecular level. The accurate determination of hydrogen positions, which is critical for this, is a requirement that neutron diffraction is uniquely suited for. Preliminary neutron diffraction experiments with these crystals conducted at the Institute Laue-Langevin (Grenoble, France) reveal diffraction to beyond 2.5 angstrom. Macromolecular crystal growth is a process involving many parameters, and statistical experimental design is naturally suited to this field. These techniques are sample independent and provide an experimental strategy to maximize crystal volume and habit for neutron diffraction studies.

Judge, R. A.↗

Organometallic Polymeric Conductors

For aerospace applications, the use of polymers can result in tremendous weight savings over metals. Suitable polymeric materials for some applications like EMI shielding, spacecraft grounding, and charge dissipation must combine high electrical conductivity with long-term environmental stability, good processability, and good mechanical properties. Recently, other investigators have reported hybrid films made from an electrically conductive polymer combined with insulating polymers. In all of these instances, the films were prepared by infiltrating an insulating polymer with a precursor for a conductive polymer (either polypyrrole or polythiophene), and oxidatively polymerizing the precursor in situ. The resulting composite films have good electrical conductivity, while overcoming the brittleness inherent in most conductive polymers. Many aerospace applications require a combination of properties. Thus, hybrid films made from polyimides or other engineering resins are of primary interest, but only if conductivities on the same order as those obtained with a polystyrene base could be obtained. Hence, a series of experiments was performed to optimize the conductivity of polyimide-based composite films. The polyimide base chosen for this study was Kapton. 3-MethylThiophene (3MT) was used for the conductive phase. Three processing variables were identified for producing these composite films, namely time, temperature, and oxidant concentration for the in situ oxidation. Statistically designed experiments were used to examine the effects of these variables and synergistic/interactive effects among variables on the electrical conductivity and mechanical strength of the films. Multiple linear regression analysis of the tensile data revealed that temperature and time have the greatest effect on maximum stress. The response surface of maximum stress vs. temperature and time (for oxidant concentration at 1.2 M) is shown. Conductivity of the composite films was measured for over 150 days in air at ambient temperature. The conductivity of the films dropped only half an order of magnitude in that time. Films aged under vacuum at ambient temperature diminished slightly in conductivity in the first day, but did not change thereafter. An experimental design approach will be applied to maximize the efficiency of the laboratory effort. The material properties (initial and long term) will also be monitored and assessed. The experimental results will add to the existing database for electrically conductive polymer materials. Attachments: 1) Synthesis Crystal Structure, and Polymerization of 1,2:5,6:9,10-Tribenzo-3,7,11,13-tetradehydro(14) annulene. 2) Reinvestigation of the Photocyclization of 1,4-Phenylene Bis(phenylmaleic anhydride): Preparation and Structure of (5)Helicene 5,6:9,10-Dianhydride. 3) Preparation and Structure Charecterization of a Platinum Catecholate Complex Containing Two 3-Ethynyltheophone Groups. and 4) Rigid-Rod Polymers Based on Noncoplanar 4,4'-Biphenyldiamines: A Review of Polymer Properties vs Configuration of Diamines.

Youngs, Wiley J.↗

Laser diode initiated detonators for space applications

Ensign Bickford Aerospace Company (EBAC) has over ten years of experience in the design and development of laser ordnance systems. Recent efforts have focused on the development of laser diode ordnance systems for space applications. Because the laser initiated detonators contain only insensitive secondary explosives, a high degree of system safety is achieved. Typical performance characteristics of a laser diode initiated detonator are described in this paper, including all-fire level, function time, and output. A finite difference model used at EBAC to predict detonator performance, is described and calculated results are compared to experimental data. Finally, the use of statistically designed experiments to evaluate performance of laser initiated detonators is discussed.

Ewick, David W.↗

Analysis of Solids Flow Rate through Nonmechanical L-Valve in an Industrial-Scale Circulating Fluidized Bed Using Group B Particles

A series of statistically designed experiments were conducted using two different Geldart Group B particles in a 0.3 m diameter circulating fluidized bed (CFB) cold model to evaluate the nonmechanical L-valve for controlling the solids flow rate. The objective of this study was to investigate the effects of standpipe aeration, L-valve aeration, solids inventory, and superficial gas velocity through the riser on the solids flow rate. A stochastic correlation was developed for calculating the solid flow rate as a function of these variables. It was found that the solid flow rate increased directly proportional to each of these variables. Dimensional analysis was used to generate an expression for the solids turnover ratio. The model developed in the present study is intended to simulate flow in the present CFB loop. In conclusion, it is not intended for scale-up and will probably not apply for alternative CFB loops with different geometries/pressure balance conditions.

42 ENGINEERING↗

Factors affecting laser-trim stability of thick film resistors

Various factors affecting precision of trim and resistor stability were considered. The influence of machine operating parameters on resistor performance was examined and quantified through statistically designed experiments for a Q switched YAG laser system. Laser kerf quality was studied by scanning electron microscopy and related to kerf isolation resistance measurements. A relatively simple production oriented, quality control test is proposed for rapid determination of kerf electrical stability. In addition, the effect of cut design and extent of trim on precision and stability were discussed.

Cote, R. E.↗