MIL-STD-1330D(SH)
20 September 1996
APPENDIX C
TEST PROCEDURE FOR SOLVENT EXTRACTION OF AN AQUEOUS INORGANIC CLEANER C.1 SCOPE
C.1.1 Scope. This appendix is a mandatory part of the standard. The information contained herein is intended for compliance. This appendix provides a procedure for solvent extraction of inorganic aqueous Navy oxygen cleaner (NOC) or tri-sodium phosphate (TSP) cleaning solution. The solvent extract is subsequently analyzed for hydrocarbon oil and grease or non-volatile residue.
C.2 APPLICABLE DOCUMENTS
This section is not applicable to this appendix. C.3 PROCEDURE
C.3.1 Summary of test method. The solvent extraction is performed by serially extracting a 500 mL homogenized sample of NOC or TSP with three 160 mL volumes of a NAVSEA approved halogenated solvent if analyzing for non-volatile residue (NVR) by gravimetric, or serially extracting a 100 mL homogenized sample of NOC or TSP with three 30 mL volumes of HCFC-225s or CFC-113 solvent if analyzing for hydrocarbon oil and grease by infrared spectrophotometry. Extracts analyzed for NVR are subsequently diluted to 500 mL, while extracts analyzed for hydrocarbon oil and grease by infrared spectrophotometry are subsequently diluted to 100 mL.
C.4 Significance and use.
C.4.1 NOC in accordance with MIL-DTL-24800 and TSP in accordance with
O-S-642 are aqueous inorganic solutions that generally contain less than 1 ppm
solvent extractable material. NOC and TSP remove industrial oils and greases by
displacement with the resultant removed insoluble contaminants existing as a
suspension. When mixed with a solvent, the solvent extracts the oil and grease
for post hydrocarbon oil and grease or NVR analysis depending upon the solvent
used.
C.4.2 All NAVSEA halogenated solvents are denser than NOC or TSP solutions so the solvent will settle to the bottom of a separatory funnel during an extraction process.
C.4.3 This test method does not acidify the NOC aqueous sample to a pH of 2 or less like common waste water analyses. Soluble organic materials that would be detectable when acidifying to a pH of 2 are easily detected as a stable foam when performing the shake test as specified in 5.13.2.2.
C.4.4 The homogenizing process cleans oil and grease from the sides of the sample container and equally distributes insoluble oil and grease through the sample as a fine emulsion. This ensures that samples drawn from the original 500 to 600 mL sample are representative.
C.4.5 During the extraction process, small quantities of aqueous cleaner solution will be captured by the solvent. The non-volatile inorganic constituents of the captured aqueous cleaner can interfere with subsequent NVR analyses. This interference can be avoided by establishing a baseline NVR analysis of the aqueous cleaner.
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