MIL-STD-1330D(SH) APPENDIX C
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b. Sample/homogenizing bottles of 1 liter volume for collecting and homogenizing NOC or TSP samples. Ensure the opening is large enough to allow insertion of the homogenizer generator (item (a)). Wide mouth glass sample bottles with external safety coatings and Teflon lined caps are acceptable, as are sampling containers manufactured from Teflon, Teflon lined glass, Teflon lined plastic, or stainless steel. Suitable containers are available from laboratory supply houses such as Thomas Scientific.
c. Graduated cylinders of 50 mL minimum volume with minimum graduations of 10 mL to measure 30 mL of solvent and 100 mL minimum volume with minimum graduations of 50 mL to measure 100 mL of aqueous sample, or 250 mL minimum volume with minimum graduations of 10 mL to measure 160 mL of solvent and 500 mL minimum volume with minimum graduations of 100 mL to measure 500 mL of aqueous sample. Cylinders should be glass.
d. Separatory funnels of 250 mL volume minimum for extracting a 100 mL aqueous sample, or 1000 mL
minimum volume for extracting a 500 mL aqueous sample. Funnels should be glass.
e. Beakers of sufficient capacity to collect 30 mL or 160 mL serial solvent extracts and transfer to the volumetric flask. Beakers should be glass.
f. Volumetric flasks, or equal, of 100 mL minimum volume with minimum graduations of 100 mL to collect the three 30 mL solvent extracts, or 500 mL minimum volume with minimum graduations of 500 mL to collect the three 160 mL solvent extracts.
C.6 Reagents.
a. Navy oxygen cleaner (NOC) in accordance with MIL-DTL-24800.
b. Tri-sodium phosphate (TSP) in accordance with O-S-642 prepared as specified in 4.3.2.
c. Hydrochloric or sulfuric acid (1+1), ACS reagent grade, prepared by slowly and carefully adding 1 volume of hydrochloric acid (HCl) or sulfuric acid (H2SO4) to 1 volume of water.
d. CFC-113 or HCFC-225 (see Appendix E). C.7 Samples.
a. A 500 to 600 mL NOC or TSP sample shall be collected for hydrocarbon or NVR determination. The sample bottles used to collect the sample shall have been cleaned as specified in C.8.
b. A 500 mL sample of homogenized NOC or TSP will be used when performing a solvent extraction for post
NVR analysis by gravimetric.
c. A 100 mL sample of homogenized NOC or TSP will be used when performing a solvent extraction for post hydrocarbon oil and grease analysis by infrared spectrophotometry.
C.8 Preparation and maintenance of apparatus.
C.8.1 When handling CFC-113 or HCFC-225, the safety precautions specified by the material safety data sheet
(MSDS) and 4.4.1 shall be followed.
C.8.2 Apparatus used in the procedure, including the sample bottles, homogenizer, homogenizing container, graduated cylinder, filtration reservoir, and demineralized water container, shall have been cleaned using a component cleaning process as specified in this standard, or equal.
C.8.3 After contact with NOC or TSP cleaning solution, all apparatus shall immediately be rinsed with demineralized water to remove residual cleaner, to prevent formation of inorganic deposits and to maintain cleanliness.
C.9 Procedure.
C.9.1 Cool the 500 to 600 mL NOC or TSP sample to room temperature or less. Acidify TSP samples to a pH
of 2 or less.
C.9.2 Homogenize the 500 to 600 mL sample for 3 minutes at a speed of about 7,500 rpm (position 3 on an
OMNI Model GLH homogenizer).
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