Stock Solution Reaction Procedure

CBI Nanosys, Inc. Milpitas, CA 95035 September 1, 2014 Page 1 of 4

LS – Laboratory Glassware Operations in Hood and

Gloveboxes to produce product

GEN II – Usage of 50 Gallon Reactor/ Mixing Tanks in a Closed

System with Transfer tanks to produce product.

End of Process End of Process
LS-C1 Add 400-613 g trioctylphosphine oxide (TOPO), 79- 138g tetradecylphosphonic acid (TDPA), and stir bar to a 3 L

5-neck RB Flask. Evacuate and refill with Nitrogen 3 times. Turn on nitrogen purge, Add 184-287 ml of Cd Stock (Cd/

TOP) using 24 ml syringes to flask. Cool to 110°C. Evacuate the flask. Hold at 110 °C under vacuum for 30 min-3 hours.

LS-C5 Remove thermocouple. Replace septa cap and addition funnels with secured glass stoppers. Bring flask into the glove-box under vacuum.

Core Reaction Procedure

CBI Nanosys, Inc. Milpitas, CA 95035 September 1, 2014 Page 2 of 4

GEN II-C1 Add 9.3-42 Kg trioctylphosphine oxide (TOPO), 1.6-9.6 Kg tetradecylphosphonic acid (TDPA), 4.3-20 L Cd

Stock in a 100 gallon reactor vessel. Heat to 250 C in 30 minutes, purge for 30-90 minutes, reduce purge and ramp

temperature to 300 C

LS – Laboratory Glassware Operations in Hood and

Gloveboxes to produce product

GEN II – Usage of100 Gallon Reactor/ Mixing Tanks in a Closed System with Transfer tanks to produce product.

End of Process End of Process
LS-C7 Pour off supernatant. Dissolve QD with TDPA

Ligands with Hexane 2-4 ml per bottle syringes out and repeated once. Collect on syringed material in one bottle. LS-C8 Prepare 1 mL sample for QAQC testing. Determine absorbance λ using the UV/vis spectrometer and emission λ and

distribution full width half max using the fluorometer. Sample is prepared in glove box, taken out in a closed cuvette to do a UV- Vis reading. In fume hood, a sample is made using wet hexane to prepare the second reading, using the fluorometer.

Core Wash Procedure

CBI Nanosys, Inc. Milpitas, CA 95035 September 1, 2014 Page 3 of 4

End of Process

GEN II-C6 TFF is operated until process meets specification;

the material is then pumped to another transfer vessel. GEN II-C7 Prepare 1 mL sample for QAQC testing. Determine absorbance λ using the UV/vis spectrometer and emission λ and distribution full width half max using the fluorometer. Sample is prepared in glove box, taken out in a closed cuvette to do a UV-Vis reading. In fume hood, a sample is made using wet hexane to prepare the second reading, using the fluorometer. End of Process
LS-C8 Laboratory glassware is placed into a 30% Potassium Hydroxide (KOH) / 70% Isopropyl Alcohol (IPA) base bath

for a minimum of thirty minutes. LS-C9 Retrieve glassware and pour off any residual base bath and gently submerge into sodium bicarbonate rinse bath to neutralize the 30% Potassium Hydroxide (KOH) /

70% Isopropyl Alcohol (IPA).

LS-C10 Retrieve glassware from neutralizer bath and place into nitric acid bath bin.

LS-C11 Place glassware in bin and transport to rinse sink. Glassware is washed minimal of two times with tap water, inspected and then rinsed with deionized water.

LS-C12 Glassware is placed on pegs to dry. If the wet

glasswear is needed hastily, it can be rinsed with ethanol and then drip dried before placing in a designated glass drying oven (100° C). Glassware is dried for a minimum of

fifteen minutes before being removed.

End of Process

LS-C13 The hot glass should be cooled in a designated area with visible warning signs for hot glassware. Once cooled and safe to handle with clean nitrile gloves, the glassware can be restocked

in appropriately labeled locations and is ready for use.

Glassware Washing and GEN II Reactor Cleaning

Nanosys, Inc. Milpitas, CA 95035 September 1, 2014 Page 4 of 4

GEN II-C8 All tanks and lines are cleaned with a clean in place system using Toluene at 50 C.

GEN II-C9 All Transfer tanks and flexible lines are taking to the stationary pumped cleaning system using Toluene. End of Process