Statement of Work Attach 2.pdf

SOW Attachment 2:

Preparation of Standard Solutions of Hydrocarbon Oils in Novec 71DE

Revision 2. Updated: 9 Jun 2021

Table 1. Equipment and Materials

Item Notes Source

Analytical Balance Readability: 0.01 mg / 0.1mg

Maximum Capacity: 61g / 220 g

Repeatability: 0.03 mg / 0.1 mg

Sensitivity Temperature Drift (10°C30°C): 2.5 ppm/°C

Built-in Adjustment Weight

Mettler Toledo, AB 265-S

Drying Oven For drying glassware Local Supply

Volumetric Pipets (various sizes) Class A in accordance with ASTM E969, Serialized & Certified, Local Supply

Volumetric Flasks (various sizes) Class A in accordance with ASTM E288, Serialized & Certified, Local Supply

Syringe (5-10 µL) with Needle For dispensing oils Local Supply

Glass Transfer/Weighing Funnel Kimble Kontes P/N 747600-0013 or similar, compatible with volumetric flask

Local Supply

Tongs Stainless steel Local Supply

Aluminum Weigh Dish (Small) Diameter: 25 mm Local Supply

Aluminum Weigh Dish (Large) Diameter: >25 mm Local Supply

Cleanroom Wipers e.g., Berkshire Durx 670 with low releasable particulates, suitable for cleanroom use

Local Supply

3M Company Novec 71DE Local Supply

Mineral Oil, pure 1 L bottle: AC415080010; CAS 8042-47-5

ACROS Organics, Fisher Scientific

MIL-PRF-5606H Synonyms: NSN 9150002526383; Royco 756;

MIL-H-5605 (cancelled)

Anderol, Local Supply

MIL-PRF-83282D Synonyms: NSN 9150001497431; Royco 782;

MIL-H-83282 (cancelled)

Anderol, Local Supply

Table 1. (cont’d)

Item Notes Source

Monoplex DOS Synonyms: Sebacate;

Decanedioic acid, di(2-ethylhexyl) ester; CAS Reg. No.

122-62-3; Di(2-ethylhexyl) sebacate, Sebacic acid di(2-ethylhexyl) ester, ‘Dioctyl’ sebacate; di-2-ethyl hexyl sebacate, ester, HallStar, Local Supply

Mobil Velocite Oil No. 10 Replacement for Exxon Spinesstic 22 (discontinued) for Fluke DWT and other

Local Supply

Lab Detergent For washing glassware Local Supply

1. Introduction and Description

This procedure provides instructions for preparing standard solutions of hydrocarbon-based oils in 3M Company Novec 71DE for developing a quantitative method for approximating the hydrocarbon concentration in unknown test solutions of this solvent.

2. Preliminary Operations

2.1. Ensure that the work area is clean, well illuminated, and that environmental conditions and controls are appropriate for preparing the solutions.

2.2. Ensure all glassware has been thoroughly cleaned with laboratory detergent, rinsed multiple times with water and deionized water, and dried.

2.2.1. Volumetric glassware may be rinsed with 99.5% Ethanol1 to aid the drying process.

2.2.2. Allow the glassware to completely dry prior to use.

2.2.3. To aid the drying process, a drying oven may be used for non-volumetric glassware. Class

A volumetric glassware (flasks and pipets) should not be oven-dried1.

3. Preparation of 2,000 PPM Stock “A” Standard Solution

These instructions are for preparing 1,000 mL of a 1,000 ppm solution of oil in Novec 71DE. These may be modified accordingly for a different amount or a different concentration of Stock “A” solution.

3.1. Record the lot number from the bottle of Novec 71DE used and the certificate of analysis (if there is an identifying number).

3.2. Rinse the inside of the large aluminum dish with Novec 71DE and allow it to dry completely.

Dispose of the rinse solvent in the suitable waste solvent container. Place the dried dish on the balance2.

1 ASTM E542, -01 (2007) Standard Practice for Calibration of Laboratory Volumetric Apparatus, §7.2 2 Using a lightweight aluminum dish is an optional precaution against spills in the event that the balance pan cannot easily removed for cleaning.

3.3. Using tongs, rinse the glass transfer/weighing funnel with Novec 71DE and allow it to dry completely. Dispose of the rinse solvent in the waste solvent container. Place the transfer/weighing funnel on the aluminum dish that is already placed on the balance. Tare the balance and allow it to stabilize.

NOTE

The transfer/weighing funnel must not be handled with gloves or bare hands, only with previously cleaned tongs.

3.4. Transfer a small amount of mineral oil to a small clean beaker. Using a glass syringe (~2 mL, also previously rinsed with Novec 71DE and dried), slowly draw up ~2 mL of mineral oil, avoiding drawing in air bubbles.

3.5. Remove excess oil from the tip of the syringe by lightly touching the oil drop (if present) to the inside of the beaker containing the oil.

3.6. Holding the syringe at an angle above the transfer/weighing funnel, weigh 1.37 g of mineral oil as closely as possible (±0.001 g).

3.7. Allow the balance to stabilize and record the actual weight.

3.8. Balance may take a couple minutes to stabilize due to the small volume and density of mineral oil.

3.9. Remove the large aluminum dish from the balance and transfer to the fume hood.

3.10. Record the serial number of a 1,000 mL Class A volumetric flask, place it in the fume hood, and fill the flask approximately half full with Novec 71DE.

3.11. Using tongs, place the funnel end of the transfer/weighing funnel into the top of the 1,000 mL volumetric flask. Using a large glass syringe3 filled with Novec 71DE, carefully and thoroughly rinse the mineral oil from the transfer/weighing funnel into the volumetric flask. Ensure that all inner surfaces of the weighing funnel have been thoroughly and repeatedly rinsed.

3.12. Remove the transfer/weighing funnel from the volumetric flask and thoroughly rinse the ground glass joint of the flask with Novec 71DE to ensure all the oil is rinsed into the flask. Stopper the flask securely.

3.13. Holding the flask and stopper securely, carefully invert the flask and mix the contents thoroughly. Repeat this process several times.

3.14. Remove the stopper and fill the flask to the line with Novec 71DE. A syringe, disposable glass Pasteur pipet, or similar device should be used to add the final amount of solvent to the line. Replace the stopper and mix thoroughly as before.

3.14.1. Transfer this solution to a clean dry screw-top glass bottle fitted with a PTFE-lined cap and label the bottle.

Stock Solution “A”

Solution Concentration

(ppm)

Amount of Oil

(g)

Amount of Novec

71DE

(mL)

Approx Vol of Oil

(mL)

Estimated Type I Error

1000 1.370 1000 1.56 0.040

3 A clean disposable glass pipet (Pasteur pipet) or a PTFE/PFA wash bottle filled with Novec 71DE may be used in place of a glass syringe.

4. Preparation of 100 PPM Stock “B” Standard Solution

These instructions are for preparing 100 mL of a 100 ppm solution of oil in Novec 71DE. As above, these steps may be modified accordingly for a different amount or a different concentration of Stock “B” solution.

4.1. Record the serial number of a 100 mL Class A volumetric flask, place it in the fume hood, and fill the flask approximately half full with Novec 71DE.

4.2. Pour approximately 20 mL of Stock “A” solution into a small clean, dry beaker.

4.3. Record the serial number of a 10 mL Class A transfer (volumetric) pipet and use a pipet bulb to withdraw several mL of Stock “A” solution into the pipet. Rinse the inside walls of the pipet with the solution and discard the rinse into an appropriate waste container.

4.4. Withdraw sufficient Stock “A” solution from the beaker into the pipet to bring the liquid level approximately 20 mm4 above the line.

4.5. Holding the pipet vertically over the beaker with the tip in contact with the inside beaker wall, slowly release the solution until the bottom of the meniscus is at the line5. After withdrawing the pipet from the beaker, do not wipe the tip of the pipet or permit it to make contact with anything until the next step.

4.6. Hold the pipet vertically with the tip inside the neck of the 100 mL volumetric flask below the bottom of the ground glass surface. With the tip of the pipet lightly touching the inside neck wall of the flask, allow the contents to run freely into the flask. After it has emptied, allow the pipet to drain for approximately 2 sec., and then carefully withdraw the tip from the inside of the flask.

4.7. Withdraw the pipet, rinse the ground glass joint of the 100 mL flask with a small amount of Novec 71DE, stopper securely and mix as with Stock “A” solution.

4.8. Remove the stopper, fill the flask to the line, re-stopper and mix as with Stock “A” solution.

4.8.1. Transfer this solution to a clean dry screw-top glass bottle fitted with a PTFE-lined cap and label the bottle.

Preparation of Stock "B" Solution

Pipet__mL of Stock

Solution A into __mL Volumetric

Flask to make __ppm

Standard

Estimated Type I Error

10 100 100 0.227

5. Preparation of remaining standard solutions.

Using the same technique described for Stock “B” solution, prepare 10 through 1 ppm standard solutions in 1 ppm increments. See the table below for guidelines to prepare these standard solutions from the Stock “B” standard solution using appropriate volumetric flasks and volumetric pipets.

4 ASTM E969-02 (2007), Standard Specification for Glass Volumetric (Transfer) Pipets, § 3.2

5 ASTM E542-01 (2007), Standard Practice for Calibration of Laboratory Volumetric Apparatus, § 9.1 to make __ppm

Standard

Pipet __mL of

Stock Solution B into a __mL

Volumetric Flask

Estimated Type I

Error (%)

10.0 10 100 0.306

9.0 9 100 0.321

8.0 8 100 0.263

7.0 7 100 0.272

6.0 6 100 0.286 5.0

5 100 0.306

4.0 4 100 0.341

3.0 6 200 0.279

2.0 2 100 0.379

1.0 2.5 250 0.339