MIL-STD-1330D(SH) APPENDIX D
20 September 1996
D.9.1.1 Weigh the 250-mL bottle and cap to the nearest 0.01 g and record the weight.
D.9.1.2 Pipette 0.5 ± 0.02 mL of MS2190TEP oil (or 0.75 ± 0.02 mL of hexane)
into the bottle and replace the cap tightly.
D.9.1.3 Weigh the bottle with cap and MS2190TEP oil (or hexane) to the nearest 0.01 g and record this weight.
D.9.1.4 Measure out 200 mL of HCFC-225s in a graduated cylinder and quickly add this to the 250-mL bottle containing the MS2190TEP oil (or hexane) and tightly recap the bottle immediately. Weigh the bottle to the nearest 0.01 g and record the weight. Mix this solution thoroughly.
D.9.1.5 Calculate the weight in grams of the MS2190TEP oil (or hexane) by subtracting the weight obtained in step D.9.1.1 from the weight measured in step D.9.1.3.
D.9.1.6 Calculate the weight in grams of the HCFC-225s by subtracting the weight obtained in step D.9.1.3 from the weight measured in step D.9.1.4 and rounding off to the nearest 0.1 g.
D.9.1.7 Calculate the mg/L of MS2190TEP oil (or hexane) in HCFC-225s (Standard A) by dividing step D.9.1.5 by step D.9.1.6 and multiplying the result by 1.55 x 106 2. This value should be between 1900 and 2900 mg/L. This standard will be used to produce solutions for preparing a calibration curve and should be tightly sealed and placed in a freezer (about 0EF - a normal household refrigerator is sufficient) when not in use.
NOTE 3: Infrared standards B, C, and D should be prepared immediately before use since over time, the HCFC-225s will evaporate from a stoppered volumetric flask.
D.9.2 Prepare three infrared standards labeled as Standards B, C, and D in the three 10-mL volumetric flasks as follows:
D.9.2.1 Into the flask labeled Standard B transfer 10 microliters of Standard A and immediately dilute to 10 mL using HCFC-225s and stopper the volumetric flask.
D.9.2.2 Repeat D.9.2.1 for the flasks labeled C and D except to flask C add
30 microliters of Standard A, and to flask D add 50 microliters of Standard A.
Remember to dilute each flask to 10 mL with HCFC-225s and immediately stopper the
volumetric flask. Also reseal the bottle containing Standard A after each portion
is taken from the bottle to minimize losses due to evaporation.
D.9.2.3 Calculate the mg of MS2190TEP oil (or hexane) per liter of HCFC-225s in Standards B, C, and D by multiplying the volume in microliters of Standard A added to each 10 mL volumetric by the concentration of Standard A in mg/L (from step D.9.1.7) and dividing that result by 10,000. Record these values for use in preparing the IR calibration curve as specified in step D.9.3.
NOTE 4: During development of the IR calibration curve, the IR cell should be thoroughly cleaned with fresh solvent and then dried prior to measuring each Standard. Do not insert the cell stopper so tightly that the solvent cannot expand during IR measurement which could cause the cell to burst.
2This factor is obtained by multiplying the density of HCFC-225s (1550 g/L at 25oC) by the conversion factor for grams to mg (1000).
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