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NASA/TM-2003-212503 Infrared Database for Process Support Materials K.E. Bennett, R.E. Boothe, and H.0.Burns Marshall Space Flight Center, Marshall Space Flight Center, Alabama June 2003

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The NASA STI Program Office...in Profile Since its founding, NASA has been dedicated to the advancement of aeronauticsand space science. The NASA Scientificand Technical Information (STI) Program Office plays a key part in helping NASA maintain this important role. The NASA STI Program Office is operated by Langley Research Center,the lead center for NASA’s scientific and technical information. The NASA STI Program Office provides access to the NASA STI Database, the largest collection of aeronautical and space science STI in the world. The Program Office is also NASA’s institutional mechanism for disseminating the results of its research and development activities.These results are published by NASA in the NASA STI Report ‘ Series,which includesthe following report types: TECHNICAL PUBLICATION. Reports of completed research or a major significant phase of research that present the results of NASA programs and include extensive data or theoretical analysis. Includes compilations of significant scientificand technical data and information deemed to be of continuing reference value. NASA’s counterpartof peer-reviewed formal professional papers but has less stringent limitations on manuscript length and extent of graphic presentations. TECHNICAL MEMORANDUM. Scientific and technical findingsthat are preliminary or of specializedinterest, e.g., quick release reports, working papers, and bibliographies that contain minimal annotation. Does not contain extensive analysis. CONTRACTOR REPORT. Scientific and technical findings by NASA-sponsored contractors and grantees. CONFERENCEPUBLICATION. Collected papers from scientific and technical conferences, symposia, seminars, or other meetings sponsored or cosponsored by NASA. SPECIAL PUBLICATION. Scientific,technical, or historical information from NASA programs, projects, and mission, often concerned with subjectshaving substantial public interest. TECHNICALTRANSLATION. English-language translations of foreign scientific and technical material pertinent to NASA’s mission. Specialized services that complement the STI Program Office’s diverse offerings include creating custom thesauri, building customized databases, organizing and publishing research results.. .even providing videos. For more information about the NASA STI Program Office, see the following: Access the NASA STI Program Home Page at http:Nwww.sti.nasa.gov E-mail your question via the Internet to help@sti.nasa.gov Fax your question to the NASA Access Help Desk at (301)621-0134 Telephone the NASA Access Help Desk at (301) 621-0390 Write to: NASA Access Help Desk NASA Center for Aerospace Information 7 121 Standard Drive Hanover, MD 21076-1320

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NASA/TM-2003-212503 Infrared Database for Process Support Materials K.E. Bennett, R.E. Boothe, and H.D. Burns Marshall Space Flight Center, Marshall Space Flight Center, Alabama National Aeronautics and Space Administration Marshall Space Flight Center MSFC, Alabama 35812 June 2003

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TRADEMARKS Trade names and trademarks are used in this report for identification only. This usage does not constitute an offkial endorsement,either expressed or implied, by the National Aeronautics and Space Administration. Available from: NASA Center for Aerospace Information 7121 Standard Drive Hanover, MD 21076-1320 (301) 621-0390 National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 (703) 487-4650 .. 11

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TABLE OF CONTENTS 1. INTRODUCTION ........................................................................................................................... 2. DESCRIPTION ............................................................................................................................... 3. RESULTS ........................................................................................................................................ 4. CONCLUSIONS ............................................................................................................................. APPENDIX A-HORIZONTAL ATTENUATED TOTAL REFLECTANCE CRYSTAL ANALYZED PRODUCTS.................................................................... 7 APPENDIX B-NICOLET 750 ANALYZED SOLVENTS/LIQUIDS ............................................. 9 APPENDIX C-DRY TRANSFERENCE TEST RESULTS ............................................................. 10 APPENDIX D-SURFACE OPTICS CORPORATION MODEL 400 SPECTROMETER ANALYZED PRODUCTS....................................................................................... 1 1 APPENDIX E-SOLVENT EXTRACTION TEST RESULTS ......................................................... 12 ... 111

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LIST OF FIGURES 1. Results of transference test shown by spectra of (a) residue from dry MAPA Professional Technic glove and (b) silicone fluid F-75 1..................................... 2. Results of transference test shown by spectra of (a) residue from dry Ansell Edmont glove and (b) paraffin wax ....................................................................... 3. Results of extraction test shown by spectra of (a) residue from denatured alcohol extraction of CRP orange nylon bagging material and (b) polyamide-1 1................. I 4. Results of extraction test shown by spectra of (a) residue from TCA extraction of Rymple cloth and (b) wax dispersion ....................................................... LIST OF TABLES I 1. Process materials and residue detected ................................................................................... 10 2. Results from solvent extraction tests ....................................................................................... 12 iv

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LIST OF ACRONYMS HATR horizontal attenuated total reflectance IR infrared MP&M Materials, Processes, and Manufacturing (Department) MSFC Marshall Space Flight Center soc400 Surface Optics Corporation Model 400 Spectrometer TCA methyl chloroform TM Technical Memorandum V

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TECHNICAL MEMORANDUM INFRARED DATABASE FOR PROCESS SUPPORT MATERIALS 1. INTRODUCTION Process support materials’ compatibility with cleaning processes is critical to ensure final hardware cleanliness and that performance requirements are met. Previous discovery of potential contaminants in process materials shows the need for incoming materials testing and establishment of a process materials database. The Contamination Control Team of the Materials, Processes, and Manufacturing (MP&M) Department at Marshall Space Flight Center (MSFC) has initiated the development of such an infrared (IR) database, called the MSFC Process Materials IR database, of the common process support materials used at MSFC. These process support materials include solvents, wiper cloths, gloves, bagging materials, etc. Testing includes evaluation of the potential of gloves, wiper cloths, and other items to transfer contamination to handled articles in the absence of solvent exposure, and the potential for solvent exposure to induce material degradation. This Technical Memorandum (TM) summarizes the initial testing completed through December 2002. It is anticipated that additional testing will be conducted with updates provided in future TMs.

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1. DESCRIPTION Materials were analyzed using two different IR techniques: (1) Dry transference and (2) liquid extraction testing. The first of these techniques utilized the Nicolet Magna 750 IR spectrometer outfitted with a horizontal attenuated total reflectance (HATR) crystal accessory. The region from 650 to 4,000 wave numbers was analyzed, and 50 scans were performed per IR spectrum. A dry transference test was conducted by applying each sample with hand pressure to the HATR crystal to first obtain a spectrum of the parent material. The material was then removed from the HATR crystal and analyzed to determine the presence of any residues. If volatile, liquid samples were examined both prior to and following evaporation. A list of materials tested by the dry transference technique can be found in appendix A; the liquid samples analyzed are listed in appendix B. Dry transference test results are shown in appendix C. The second technique was to perform an extraction test with each sample in five different solvents. The materials used for extraction testing were those most common in MP&M laboratories and the substore in building 4707. A list of these materials can be found in appendix D. The extraction residues were scanned using a Surface Optics Corporation 400 spectrometer (SOC400) outfitted with i a V-sphere analysis accessory. The analysis region for this instrument was 650 to 4,000 wave numbers, and 32 scans were performed per IR spectrum. Each sample material was tested a total of 10 times (2 exposure periods with each of the 5 solvents). For the first portion of the test, a sample would be agitated in the solvent for 10 s in a glass jar. The solvent would then be added to the V-sphere cup, allowed to evaporate, and then scanned. For the second exposure period, a sample would be placed in a I glass jar with the solvent for a total of 1 hr. The solvent would then be added to the V-sphere cup, allowed to evaporate, and then scanned. Extraction test results are shown in appendix E. Once the scans were complete for both the dry transference and the extraction tests, the residue from each scan was interpreted. Several very significant findings were made using both techniques. 2

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1. RESULTS Dry transference testing was important for all materials since gloves are used for handling, wiper cloths can be used for dry cleaning, and plastic forms are used for bagging contact hardware. Glove selection is critical since direct contact with sensitive hardware occurs during handling. Two gloves tested using the transference test were found to contain a silicone coating. A few different lots of each of these gloves were tested to determine the accuracy of the findings. The gloves found to include the silicone residue were the MAPA Professional Technic@glove and the Microflex@Ultra One@latex glove. In each case it is believed that the silicone is a coating on the glove and not a degradation product or glove particulate. Spectra of the MAPA Professional Technic glove residue and a common silicone are shown in figure 1. 0.006 0.004 0.002 0 P) -0.002 u em -0.004 e0 1.o m s 0.8 0.6 0.4 0.2 0 Wave Numbers (cm-') Figure 1. Results of transference test shown by spectra of (a) residue from dry MAPA Professional Technic glove and (b) silicone fluid F-75 1. Residue collected from dry transference testing of Ansell Edmont gloves was shown to be consistent with a hydrocarbon wax such as paraffin (fig. 2). This residue is believed to be a coating on the glove and not a degradation product or glove particulate. 3

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0.070 0.060 0.050 0.040 0.030 0 0.020 2 0.010 Al 0 g 1.0 (A s 0.8 0.6 0.4 0.2 1 3,500 3000 2,500 2,d00 1 ,io0 1,000 5 Wave Numbers (cm-l) Figure 2. Results of transference test shown by spectra of (a) residue from dry Ansell Edmont glove and (b) paraffin wax. Extraction testing was conducted on wiper cloths, gloves, and other materials that might come in contact with solvents or solutions during cleaning processes or by inadvertent contact. The extraction testing found several significant findings as well. Tests completed on CRP orange nylon bagging material with the solvents alcohol, methyl chloroform (TCA), and acetone produced a polyamide. Dry transference testing performed on the bagging material resulted in no residue observed. This comparison indicates that the residue is a degradation product of the material. Spectra of the extraction residue and a common polyamide are shown in figure 3. 3,500 3,000 2,500 2,000 1,500 1,000 Wave Numbers (cm-l) Figure 3. Results of extraction test shown by spectra of (a) residue from denatured alcohol extraction of CRP orange nylon bagging material and (b) polyamide-1 1. 4 I I

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_ - Another finding from the extraction testing is that exposure of Rymple cloth to TCA and alcohol residue produces a hydrocarbon wax residue. When performing dry transference testing on the HATR crystal, the residue from the Rymple cloth was a fiber residue, indicating that the extraction residue is a degradation product. Spectra of the Rymple cloth residue and a common hydrocarbon wax are shown in figure 4. 3,500 3,000 2,500 2,000 1,500 1,000 Wave Numbers (cm-') Figure 4. Results of extraction test shown by spectra of (a) residue from TCA extraction of Rymple cloth and (b) wax dispersion. 5

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1. CONCLUSIONS The test results summarized in this TM illustrate that many process support materials in use in MSFC laboratories have the potential to transfer contamination to items with which they come into contact. This is particularly true if the material is used in conjunction with a solvent. Continued cataloguing of processing materials will increase the likelihood that unknown contaminants found on bonding, optical, and other surfaces can be accurately identified. The database can also serve as a reference to help determine how or whether processing materials should be used for specific applications. 6 I

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APPENDIX A-HORIZONTAL ATTENUATED TOTAL REFLECTANCE CRYSTAL ANALYZED PRODUCTS The following are products analyzed using the HATR crysal accessory: Gloves: Ansell Chem-WhiteTM glove Ansell Edmont Chem-WhiteTM Sol-Vex@nitrile glove 37-105 Ansell Edmont Sol-Vex@glove 9323A 37-1 55 8 Ansell Nitrilite@gloves lot 0103501008 Berkshire BCR@glove liner Cotton glove insert MAPA Pioneer Stanzoil@neoprene glove MAPA Professional Technic@glove NS-35 Microflex@Ultra One@glove ORS treated industrial glove RN67368 Wipers: Anticon lOO@wiper cloth by Milliken Research Corporation Anticon lOO@with Plus-4 premoistened wiper cloth by Milliken Research Corporation Chix@TM aerospace wiper Contec@wiper Horizon tech wipe 530/5353 Merocel@wiper cloth 900284 Multigraphics@Multilith@pads 200-847 PF degreaser solvent wiper Rippey wiper cloth Ross optical lens tissue Rymple cloth Vera Clean premoistened actone wipes lot 071902 Brushes: Maxwell Corp. of America 2-in foam brush Sponge brush 828265 Tynex brush part No. 01-004210-001 Cleaners: Blue Gold industrial cleaner by Modern Chemical Inc. ChemCo 030 white titanium dioxide LS06838 I Cole-Panner lab cleaning solution series 8790 DIF hand cleaner type 1C12 grade B I 7

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Miscellaneous: 2100 blue side 2100 brown side Brown paper Capran@980 Cotton-tippedapplicator CRC Power Lube@ CRP orange nylon bag DoAll rust preventive DOW Corning@RTV sealant Kapton@H Polyethylene bag Silikroil@by Kano Laboratories Techspray Envi-ro-techTMcircuit chiller 1672 TriFlow mold release by Krylon WD- 40@

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APPENDIX B-NICOLET 750 ANALYZED SOLVENTS/LIQUIDS The following are solvents and liquids analyzed using the Nicolet 750 spectrometerconfigured as described in section 2: Blue Gold industrial cleaner by Modern Chemical Inc. Cole-Parmer lab cleaning solution series 8790 Dichloromethane alpha E-Z lacquer thinner Fisher Scientificmethyl ethyl ketone UN1193 HFE-7100 Novec, 3M lot 24132 Humco Isopropyl Rubbing Alcohol 70% USP Klean-Strip S-L-X denatured alcohol Lacquer thinner Mallinckrodt acetone SpectrAR 2438 Methyl ethyl ketone PF degreaser RE-ENTRY@Plus-4 by Petroferm Inc. Silquest A-1 87 Toluene Xylene dyce 9

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APPENDIX C-DRY TRANSFERENCE TEST RESULTS Table 1 shows process materials used and whether residue was detected as a result of dry transference testing. Table 1. Process materials and residue detected. Process Material 2100 blue side 2100 brown side Ansell Chem-White glove Residue Detected Ansell Edrnont Chern-White Sol-Vex nitrile glove 37-106 Ansell Edmont gloves Ansell Edmont Sol-Vex glove 9323A 37-155 8 Ansell Nitrilite gloves Anticon 100 wiper cloth by Milliken Research Corp. Anticon 100 wiper with Plus 4 by Milliken Research Corp. Berkshire BCR glove liner Brown paper Capran980 Chix TM aerospace wiper Contec wipe Cotton glove insert Cotton-tipped applicator CRC Power Lube CRP orange nylon bag DoAll rust preventive Horizon tech wipe 5350/5353 Kapton H X X X X MAPA Pioneer Stanzoil neoprene glove NS-35 X MAPA ProfessionalTechnic glove NS-35 X Maxwell Corp. of America 2-in foam brush Merocel wiper cloth 900284 Microflex Ultra One glove Multigraphics Multilith pads ORS treated industrial glove RN67368 PF degreaser solvent wiper Polyethylenebag Rippey wiper cloth Ross optical lens tissue Silikroil by Kano Laboratories Sponge brush 828265 TriFlow mold release by Krylon Tynex brush pari No. 01-004210-001 Vera Clean acetonewipes WD-40 X = Dry transference residue 10 i X X X

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APPENDIX D-SURFACE OPTICS CORPORATION MODEL 400 SPECTROMETER ANALYZED PRODUCTS The following are products analyzed in liquid extraction testing using the SOC-400 spectrometer configured as described in section 2: Solvents used: Acetone Denatured alcohol Ethanol Isopropyl alcohol TCA Products analyzed: 2100 (brown and blue sides) Ansell nitrile glove lot 0103501008 Ansell Sol-vex Ansell Sol-vex 9323A 37-1 558 0493 Anticon 100 wiper by Milliken Research Corporation Capran 980 Clean class PFLT203 lot 4587 Contec wiper CRP orange nylon bag Horizon tech wipes 5350/5353 Kapton H MAPA Pioneer Stanzoil neoprene glove NS-35 Merocel wiper cloth 900284 Microflex latex glove Microflex Ultra One glove UL-3 15-XL Multigraphics Multilith pads 200-847 Polyethylene bag Rippey wiper cloth Ross optical lens tissue Rymple cloth 11

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APPENDIX E-SOLVENT EXTRACTION TEST RESULTS Results from solvent extraction tests are shown in table 2. Table 2. Results from solvent extraction tests. Process Material Acetone Solvent Denatured Isopropyl Alcohol Ethanol Alcohol TCA - - - - - - - 7 - - - -10 s -1 hr -10 s -1 hr -10s -1 hr -10 s -1 hr 10 s 1 hr 2100 Bagging material X X Ansell nitrile glove X X Ansell Sol-vex glove X X Anticon 100 wiper cloth X X Capran 980 X X Clean class glove X X Contec wiper cloth X X CRP nylon bagging material X X Horizon tech wipe Kapton H MAPA Pioneer Stanzoil neoprene glove X X Merocel wiper cloth X Microflex latex gloves X X Microflex Ultra One latex glove X X Multigraphics Multilith pads Polyethylene bag X X Rippey wiper cloth X X Ross optical lens tissue Rymple cloth X X - X = Extraction residue observed X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X X - -

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Form Approved REPORT DOCUMENTATION PAGE 1 OMB NO.0704-0188 I Public reportingburdenfor this colleciionof inlormationis estimatedto average 1 hour per response, indudingthe time for reviewinginstructins. searchingexistingdata sources, gatherlngand maintainingthe data needed, and completingand reviewingthe colleclin 01 informah. Send comments regardingthis burden estimate or any other ZSPecIof this cdle*ion of information.includingsylgestiw lor reducing ma burden,to Washington HeadquartersServices.Directoratelor lnformabn Operalion and Reports.1215 Jefferson Davis Highway. Suae 1204.Arlington, VA 222024302, and to the officed Managementand Budget, Papetwork ReductionProject (0704-0188),Washington, DC 20503 1. AGEN6 USE ONLY (Gave Blank) 2. REPORTDATE June 2003 7. PERFORMINGORGANIZATION NAMES(S) AND ADDREWES) George C. Marshall SpaceFlight Center Marshall SpaceFlight Center, AL 35812 I 3. REPORTTYPE AND DATESCOVERED Technical Memorandum 0. PERFORMING ORGANIZATION REPORT NUMBER M-1078 9. SPONSORING/MONITORINGAGENCY NAME(S) AND ADDRESqES) 10. SPONSORINGIMONITORING National Aeronauticsand Space Administration Washington, DC 205464001 11. SUPPLEMENTARYNOTES AGENCY REPORTNUMBER NASA/TM--2003-2 12503 Prepared by the Materials, Processes, and Manufacturing Department, Engineering Directorate I i2a DISTRIBUTIOWAVAILAB~UTYSTATEMENT Unclassified-Unlimited SubjectCategory 23 rNonstandard Distribution 13. ABSTRACT (Maximum200 words) 12b. DISTRIBUTIONCODE I In order to help identify contamination found on bonding surfaces, optical surfaces, or other items, the Materials Contamination Team of the Materials, Processes, and Manufacturing Department at Marshall Space Flight Center (MSFC) has initiated the development of an infrared database containing MSFC process materials and residues. Process materials analyzed to date using infrared spectroscopy for transferable and extractable contamination have included gloves, wiper cloths, solvents, bagging materials, etc. Significant findings included silicone contamination on several gloves and observations of extractables from the majority of materials tested. ~ ~~ 14. SUBJECTTERMS 15. NUMBER OF PAGES infrared spectroscopy,contamination,process support materials r 18. SECURITY CLASSIFICATION 19. SECURITY CLASSIFICATION 20. LIMITATION OF ABSTRACl 17. SECURITY CLASSIFICATION OF REPORT OF THIS PAGE Unclassified Unclassified OF ABSTRACT Unclassified Unlimited