MIL-STD-1330D(SH)
20 September 1996
5.13.2.5 Solvent non-volatile residue. Non-volatile residue (NVR) of
solvent extract shall be determined in accordance with ASTM F 331 (see 6.3). This
method evaporates 500 mL of solvent to 20 to 30 mL using a rotary flash
evaporator, evaporates the 20 to 30 mL residue with a 105 to 110EC oven, cools the sample, and then weighs the remaining residue, recording the NVR in ppm. Because of the volume, expense, and effluent discharge associated with the solvent NVR analysis, activities should implement methods to collect and recycle evaporated solvent.
5.13.2.6 Solvent infrared spectrophotometry. As specified in appendix D, dichloropentafluoropropane (HCFC-225s) solvent extract can be analyzed for the presence of hydrocarbon oil and grease using a Fourier transform infrared (FTIR) spectrophotometer. Hydrocarbon oil and grease in trichlorotrifluoroethane (CFC-
113) shall be determined in accordance with ASTM D 3921 (see 6.3).
5.13.3 Particulate inspection methods.
5.13.3.1 Applicability. Unless otherwise specified, a white light visual particle inspection as specified in 5.13.3.2 shall be performed on a sample of the final rinse water or solvent. For critical applications, a particle count as specified in 5.13.3.3 shall be performed on a sample of the final rinse water or solvent.
5.13.3.2 White light visual particle inspection. Samples of final rinse water or solvent shall be visually inspected for particulate contamination. Inspection shall be performed by a person with normal visual acuity, natural or corrected, under bright white light of at least 100 foot-candles. A general purpose two D-cell flashlight, in good condition, at a distance of not greater than 18 inches directly above a surface will illuminate the surface with an intensity of not less than 100 foot-candles. Samples shall be inspected in a chemically compatible clear container or clean white dish. Any visible particles shall be cause for rejection. This visual inspection corresponds to a quantitative limit of no particles greater than 50 micrometers.
5.13.3.3 Particle count. Particle counts of final rinse water or solvent samples should meet MIL-STD-1246 cleanliness level 100 or 200 when determined in accordance with ASTM F 311 (see 6.3). A particle count is determined by filtering a sample of rinse water or solvent through a 1.0 micrometer, or less, membrane filter. The size and quantity of particles on the filter is then determined using a microscope. The particle count should be reported in relation to a known volume (1 liter) or surface area [1 square foot (ft2)] using the appropriate MIL-STD-1246 cleanliness level distribution. Note that the analysis should be performed in a clean environment to prevent contamination. One alternative to simplify the particle count is to look for a particle larger than the largest particle size allowed to have an unlimited quantity. As an example, if the largest particle
size allowed to have an unlimited quantity is 50 micrometers, look only for particles greater than 50 micrometers. A complete particle count would be required only if particles greater than 50 micrometers were observed.
5.13.4 pH analysis.
5.13.4.1 Applicability. When specified, the pH of rinse water shall be determined as specified in 5.13.4.2. The pH of NOC should be determined as specified in 5.13.4.3.
5.13.4.2 Rinse water pH. When specified, the pH of rinse water shall be determined using a pH probe, litmus paper, or phenolphthalein indicator solution. Three drops of phenolphthalein indicator solution in a 100 mL sample will appear colorless or a very slight pink when the pH is 8.0 or less.
5.13.4.3 NOC pH. To accurately measure the pH of NOC, measure pH as specified by MIL-DTL-24800, or measure in accordance with ASTM E 70 and the following:
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