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Photometric analyzer measures NVR /nonvolatile residue/ in trichloroethylene and other organic solvents. The analyzer converts the liquid solvent to aerosol and passes it between an optically focused light beam and a photodetector that is connected to standard amplifying and readout equipment.
Automatic measurement of nonvolatile residue of cleaning solvents
A protocol has been devised for formulating low-vapor-pressure precursors for protective and conversion coatings on metallic and ceramic substrates. The ingredients of a precursor to which the protocol applies include additives with phosphate esters, or aryl phosphate esters in solution. Additives can include iron, chromium, and/or other transition metals. Alternative or additional additives can include magnesium compounds to facilitate growth of films on substrates that do not contain magnesium. Formulation of a precursor begins with mixing of the ingredients into a high-vapor-pressure solvent to form a homogeneous solution. Then the solvent is extracted from the solution by evaporation - aided, if necessary, by vacuum and/or slight heating. The solvent is deemed to be completely extracted when the viscosity of the remaining solution closely resembles the viscosity of the phosphate ester or aryl phosphate ester. In addition, satisfactory removal of the solvent can be verified by means of a differential scanning calorimetry essay: the absence of endothermic processes for temperatures below 150 C would indicate that the residual solvent has been eliminated from the solution beyond a detectable dilution level.
A variety of environmental, safety, and health concerns exist over use of chlorinated and fluorinated cleaning solvents. Sandia National Laboratories, Lawrence Livermore National Laboratories, and the Kansas City Division of AlliedSignal have combined efforts to focus on finding alternative cleaning solvents and processes which are effective, environmentally safe, and compliant with local, state, and federal regulations. An alternative solvent has been identified, qualified, and implemented into production of complex electronic assemblies, where aqueous and semi-aqueous cleaning processes are not allowed. Extensive compatibility studies were performed with components, piece-parts, and materials. Electrical testing and accelerated aging were used to screen for detrimental, long-term effects. A terpene, d-limonene, was selected as the solvent of choice, and it was found to be compatible with the components and materials tested. A brief history of the overall project will be presented, along with representative cleaning efficiency results, compatibility results, and residual solvent data. The electronics industry is constantly searching for proven methods and environmentally-safe materials to use in manufacturing processes. The information in this presentation will provide another option to consider on future projects for applications requiring high levels of quality, reliability, and cleanliness from non-aqueous cleaning processes.
A microfluidic system has been designed to survive spaceflight and to function autonomously on the Martian surface. It manipulates microscopic quantities of liquid water and performs chemical analyses on these samples to assay for the presence of molecules associated with past or present living processes. This technology lies at the core of the Urey Instrument, which is scheduled for inclusion on the Pasteur Payload of the ESA ExoMars rover mission in 2013. Fabrication processes have been developed to make the microfabricated Teflon-AF microfluidic diaphragm pumps capable of surviving extreme temperature excursions before and after exposure to liquid water. Two glass wafers are etched with features and a continuous Teflon membrane is sandwiched between them (see figure). Single valves are constructed using this geometry. The microfabricated devices are then post processed by heating the assembled device while applying pneumatic pressure to force the Teflon diaphragm against the valve seat while it is softened. After cooling the device, the embossed membrane retains this new shape. This solves previous problems with bubble introduction into the fluid flow where deformations of the membrane at the valve seat occurred during device bonding at elevated temperatures (100-150 C). The use of laminated membranes containing commercial Teflon AF 2400 sheet sandwiched between spun Teflon AF 1600 layers performed best, and were less gas permeable than Teflon AF 1600 membranes on their own. Spinning Teflon AF 1600 solution (6 percent in FLOURINERT(Registered TradeMark) FC40 solvent, 3M Company) at 500 rpm for 1.5 seconds, followed by 1,000 rpm for 3 seconds onto Borofloat glass wafers, results in a 10-micron-thick film of extremely smooth Teflon AF. This spinning process is repeated several times on flat, blank, glass wafers in order to gradually build a thick, smooth membrane. After running this process at least five times, the wafer and Teflon coating are heated under vacuum at 220 C for one hour in order to drive off any residual solvent present in the composite film. After this, a second blank, glass wafer is brought down from above and the stack is held under vacuum at 3 atm mechanical pressure for ten 10 hours.
The detailed characterization of an experimental thermoplastic polyimidesulfone adhesive based on 3,3 prime-diaminodiphenylsulfone and 3,3 prime,4,4 prime-benzophenone tetracarboxylic dianhydride was studied. Model compounds were also examined. Thermal cyclization of the amide-acid to the imide was studied by a variety of techniques including DSC, TGA, MS, in situ diffuse reflectance-FTIR, and flow mearsurement. Characterizations were continued during the processing of adhesive tapes and the fabrication, bonding, and testing of lap shear specimens. Results provide fundamental insights into the role of cure chemistry, and the effects of residual solvent and volatile produces on processing and performance. These insights and the resulting chemical models should lead to more efficient processing cycles for these and other related thermoplastic adhesive systems.
The requirements for repair work on Naval aircraft composite wing skins that can be performed under depot conditions (or still worse, under field conditions) are quite restrictive. Equipment that can be used is rather limited as are the available repair space and time. The procedures must be simple enough so that they can be performed satisfactorily by personnel without special knowledge in composite materials technology. Repairs of small holes should not require more than perhaps a short predrying cycle (with heat guns) and a subsequent patch bonding using a heating blanket, held in place by applying a vacuum. However, it has been observed during simulated experimental repair work that the glue lines frequently show a high content of pores and bubbles which are attributed to evaporation of moisture during the curing cycle. (Of course, other volatile materials such as residual solvent would act similarly). The purpose of this paper is to give some detailed analysis of the problem of moisture transport as a function of repair conditions, and to discuss some preliminary work to reduce the effect of moisture by removing moisture chemically with carbodiimides before it reaches a critical level for bubble formations.
The detailed characterization of an experimental thermoplastic polyimidesulfane adhesive based on 3,3 prime-diaminodiphenylsulfone and 3,3 prime,4,4 prime-benzophenone tetracarboxylic dianhydride was studied. Model compounds were also examined. Thermal cyclization of the amide-acid to the imide was studied by a variety of techniques including DSC, TGA, MS, in situ diffuse reflectance-FTIR, and flow measurement. Characterizations were continued during the processing of adhesive tapes and the fabrication, bonding, and testing of lap shear specimens. Results provide fundamental insights into the role of cure chemistry, and the effects of residual solvent and volatile produces on processing and performance. These insights and the resulting chemical models should lead to more efficient processing cycles for these and other related thermoplastic adhesive systems.
An in situ NDE dielectric impedance measurement method has been developed for ascertaining the cure processing properties of high temperature advanced thermoplastic and thermosetting resins, using continuous frequency-dependent measurements and analyses of complex permittivity over 9 orders of magnitude and 6 decades of frequency at temperatures up to 400 C. Both ionic and Debye-like dipolar relaxation processes are monitored. Attention is given to LARC-TPI, PEEK, and poly(arylene ether) resins' viscosity, glass transition temperature, recrystallization, and residual solvent content and evolution properties.
Treatment with monatomic oxygen activates surfaces of biomedical and biotechnical materials without adversely affecting properties of bulk and without introducing toxic or otherwise dangerous solvent residues. Treatment used to create carpetlike texture increasing surface area and encouraging cells to adhere and grow. On silicone tubing for vascular implants, carpet surface improves acceptance by body. On polymer beads and vessels, surface increases effectiveness of growing, storing, and separating cell cultures. Monatomic oxygen relatively abundant in upper atmosphere of Earth, thus treatments carried out on Space Shuttle missions. Alternatively, one of several high-energy neutral-beam devices used in terrestrial laboratories.
A significant increase in the use of composite materials has occurred during the past 20 years. Associated with this increased use is the potential for employees to be exposed to offgassing components from composite systems. Various components in composite systems, particularly residual solvents, offgas under various conditions. The potential for offgassing to occur increases as a composite material is heated either during cure or during lay-up operations. Various techniques can be employed to evaluate the offgassing characteristics of a composite system. A joint effort between AIA and SACMA resulted in the drafting of a proposed test method for evaluating the offgassing potential of composite materials. The purpose of testing composite materials for offgassing is to provide the industrial hygienist with information which can be used to assess the safety of the workplace. This paper outlines the proposed test method and presents round robin testing data associated with the test method. Also in this presentation is a discussion of classes of compounds which require specialized sampling techniques.
High quality films, preimpregnated tape (prepegs), and composites have been fabricated from polyimide precursor 'saltlike' solutions. These salt-like solutions have a low viscosity (5,000 to 10,000 cp) and a high solids content (50-65% by weight) and can be coated onto reinforcing fiber to produce prepegs with excellent tack and drape at 12-15% residual solvent (approximately 4-6% water from thermal imidization reaction). The processing of these types of prepegs significantly overcomes solvent removal problems and allows excellent fiber wet out. In addition, the physical characteristics of the polyimide precursor salt-like solutions permits processing into high-performance materials through the use of standard prepregging and composite fabrication equipment. The resultant composites are of high quality.
Novel aromatic/aliphatic polyimides were prepared from 2,7-diamino-9,9'- dioctylfluorene (AFDA) and aromatic dianhydrides. Upon investigating the effectiveness of these polyimides for dispersing single wall carbon nanotubes (SWNTs) in solution, three were discovered to disperse SWNTs in N,N-dimethylacetamide (DMAc). Two of these polyimides, one from 3,3',4,4'-oxydiphthalic anhydride (ODPA) and one from symmetric 3,3',4,4'-biphenyltetracarboxylic dianhydride (s-BPDA), were used to prepare nanocomposites. Homogeneous polyimide/SWNT suspensions from both polymers were used in the preparation of films and fibers containing up to 1 wt% SWNTs. The samples were thermally treated to remove residual solvent and the films were characterized for SWNT dispersion by optical and high resolution scanning electron microscopy (HRSEM). Electrical and mechanical properties of the films were also determined. Electrospun fibers were examined by HRSEM to characterize SWNT alignment and orientation.
Solvent Purity Meter /SPM/ automatically measures the soluble residue in volatile solvents used in cleaning or extraction of oils, greases, and other nonvolatile materials. The SPM gives instantaneous and continuous readout of soluble contaminant residues in concentrations as low as one part per million of solution.
Gloves are often used to prevent the contamination of critical surfaces during handling. The type of glove chosen for use should be the glove that produces the least amount of non-volatile residue (NVR). This paper covers the analysis of polyethylene, nitrile, latex, vinyl, and polyurethane gloves using the contact transfer and gravimetric determination methods covered in the NASA GSFC work instruction Gravimetric Determination and Contact Transfer of Non-volatile Residue (NVR) in Cleanroom Glove Samples, 541-WI-5330.1.21 and in the ASTM Standard E-1731M-95, Standard Test Method for Gravimetric Determination of Non-Volatile Residue from Cleanroom Gloves. The tests performed focus on contamination of critical surfaces at the molecular level. The study found that for the most part, all of the gloves performed equally well in the contact transfer testing. However, the polyethylene gloves performed the best in the gravimetric determination testing, and therefore should be used whenever solvent contact is a possibility. The nitrile gloves may be used as a substitute for latex gloves when latex sensitivity is an issue. The use of vinyl gloves should be avoided, especially if solvent contact is a possibility. A glove database will be established by Goddard Space Flight Center (GSFC) Code 541 to compile the results from future testing of new gloves and different glove lots.
We endeavor to develop and implement methods in our laboratory to convert and extract insoluble organic materials (IOM) from low car-bon bearing meteorites (such as ordinary chondrites) and Precambrian terrestrial rocks for the purpose of determining IOM structure and prebiotic chemistries preserved in these types of samples. The general scheme of converting and extracting IOM in samples is summarized in Figure 1. First, powdered samples are solvent extracted in a micro-Soxhlet apparatus multiple times using solvents ranging from non-polar to polar (hexane - non-polar, dichloromethane - non-polar to polar, methanol - polar protic, and acetonitrile - polar aprotic). Second, solid residue from solvent extractions is processed using strong acids, hydrochloric and hydrofluoric, to dissolve minerals and isolate IOM. Third, the isolated IOM is subjected to both thermal (pyrolysis) and chemical (oxidation) degradation to release compounds from the macromolecular material. Finally, products from oxidation and pyrolysis are analyzed by gas chromatography - mass spectrometry (GCMS). We are working toward an integrated method and analysis scheme that will allow us to determine prebiotic chemistries in ordinary chondrites and Precambrian terrestrial rocks. Powerful techniques that we are including are stepwise, flash, and gradual pyrolysis and ruthenium tetroxide oxidation. More details of the integrated scheme will be presented.
This slide presentation reviews the testing for Non-Volatile Residue contamination transferred to surfaces from handling and solvent cleaning. Included in the presentation is a list of the items tested, formal work instructions dealing with NVR. There is an explanation of the Gravimetric determination method used to test the NVR in a variety of items, i.e., Gloves, Swabs, Garments, Bagging material, film and Wipes. Another method to test for contamination from NVR is the contact transfer method. The use of this method for testing gloves, garments, bagging material and film is explained. Certain equations use in NVR analysis and the use of a database for testing of NVR in consumables are reviewed.
Aerospace requirements have engendered the need for instruments for automatic determination of trace impurities in liquid and gaseous systems by in-line continuous operation. These include devices for the automatic sizing and counting of minute particles (below 0.1 mm) is closed liquid and gaseous systems, and the automatic determination of nonvolatile residue in solvents and traces of hydrocarbons dissolved or dispersed in gaseous systems. The principle of operation, and characteristics of instruments, as well as results of experimental testing, are briefly described. Potential industrial applications are also suggested.