MIL-STD-1330D(SH) APPENDIX D
20 September 1996
D.5 Apparatus.
(a) A balance accurate to 0.01 g and zero drift less than 0.02 g with a capacity of at least 1000 g. The balance shall be calibrated in accordance with the Navy Metrology and Calibration Program.
Between calibrations the balance shall be verified using certified balance weights. Suitable balances such as OHAUS Model TP-2K or DENVER INSTRUMENTS Model XL-1810 are available through scientific supply houses such as Fischer Scientific.
(b) Graduated cylinders of 1000 mL and 250 mL volume. Cylinders should be glass.
(c) An infrared spectrometer, Fourier transform or equivalent instrumentation, capable of measuring absorbance differences of
0.003 optical density units (ODU) with a background absorbance of
1.30 ODU (equivalent to 5 percent transmittance) with a signal to
noise of at least 5:1 from 2955 cm-1
(3.69 micrometer).
(3.38 micrometer) to 2710 cm-1
(d) A quartz cell, IR quartz, of 10 mm pathlength with tapered Teflon stopper.
(e) Volumetric flasks, quantity three of 10 mL for preparation of infrared standards and quantity one of 100 mL, for each sample analyzed during any one period of time. Flasks should be glass.
(f) Pipet of 1 mL, graduated in 1/100 mL.
(g) Eppendorf pipet of 10 to 100 microliter, adjustable.
(h) Glass bottle for Standard A, 250 mL capacity with Teflon lined
screw cap.
(i) Refrigerator with a freezer section maintaining a temperature of
0 ± 7EF.
D.6 Reagents.
(a) MS2190-TEP in accordance with MIL-L-17331. (b) Hexane (C6H14), HPLC grade.
(c) HCFC-225s (see appendix E).
D.7 Samples.
(a) Samples of HCFC-225s used as a final cleaning solvent shall be not less than 10 mL in a glass bottle with a screw cap having a Teflon liner.
(b) Samples of HCFC-225s used to extract hydrocarbon oil and grease from aqueous samples shall be as specified in appendix C.
D.8 Preparation and maintenance of apparatus.
D.8.1 When handling HCFC-225s, the safety precautions specified by the material safety data sheet (MSDS) and 4.4.1 shall be followed.
D.8.2 Apparatus used in the procedure, including the sample bottles, IR cells, graduated cylinders, bottles and volumetric flasks shall have been cleaned using a cleaning process as specified in this standard, or equal.
D.9 Calibration.
NOTE 1: A choice of two calibration species is available to the analyst. The preferred material is MS2190TEP, a common shipboard lubricating oil. An alternative calibration species is hexane, a short chain saturated hydrocarbon which mimics the signature of many petroleum products.
D.9.1 Prepare a calibration standard labeled as Standard A of approximately
2400 mg/L of MS2190TEP oil (or hexane) in HCFC-225s as follows:
NOTE 2: All operations with HCFC-225s and hexane should be done quickly whenever the bottles or flasks holding these fluids are not tightly sealed in order to minimize losses due to evaporation of these highly volatile materials.
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