## Cover Letter

Jim Alwood, (202) 564-8974 The following is our PMN submittal for {LOREX X-14-1 - Dodecanoic acid, reaction products with cadmium zinc selenide sulfide and oleylamine Per 10-7-14 Discussion Summary of LoRex Testing Follow-up for X-14-0001 /0002 (Originally Items 1-5) Revised follow-up testing plan as follows: 1) Transmission electron microscopy for size, shape analysis and size distribution of the nanoparticles provide images. 2) X-ray diffraction of the nanoparticles for presence of crystalline phases. 3) Surface chemistry, including elemental composition, by XPS. Attachment 2 contains the results for 1-3 4) Weathering test for final product encapsulated in silicone polymer per separate discussion/sample set. Note: We have provided additional testing data per our conversation on 10/20 and includes 3M test data as well as the methodologies used. This data was submitted with our PMN Submission Report Number NANO141022466853487 for updating LOREX X-14-2. After you have had time to review we would like to set up a conference call to review and answer any questions. Thanks, Troy Troy Christensen, PE Otis Institute, Inc. 415-734-0186

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### Pay.gov Tracking ID: 25HTFKSL Agency Tracking ID: 74689549320 NANO141022147946419 201406

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Page 3 SANITIZED SUBMISSIONTony Soriano Director, Equipment Engineering & Facilities Nanosys 233 South Hillview Drive Milpitas CA 95035 tsoriano@nanosysinc.com Troy Christensen Managing Principal Otis Institute, Inc. 185 Berry Street #5509 San Francisco CA 94107 troy@otisinstitute.com 415-734-0186

Bob Dubrow Director of Chemistry Nanosys 233 South Hillview Drive Milpitas CA 95035 bdubrow@nanosysinc.com 408-240-6711



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## X 380885 CAS_Page Intentionally Blank.pdf 

### unspecified See Attachment 010 (Chemical Structure Diagram - GEN II QD Shell - Blank.pdf)

Chemical Structure Diagram - GEN II QD Shell - Blank.pdf Page 5 SANITIZED SUBMISSIONXXX

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Page 6 SANITIZED SUBMISSIONPage 7 SANITIZED SUBMISSIONPage 8 SANITIZED SUBMISSIONQuantum Dot with LA and Amine Ligands

Quantum Dot Shell Growth Solution

Cadmium selenide zinc sulfide dodecanoic acid and amine

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### XXX XXX 

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X See continuation page. id: <P7SC2bC1> Precourser component to make an optical down converter in the next step of manufacturing. 100 XXX 

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Page 10 SANITIZED SUBMISSIONP7SC2bC1 Part I, Section C, 2.b. Generic use description

The Quantum Dot Matrix material is composed of high efficiency quantum dot phosphors. Larger than a water molecule, but smaller than a virus, these tiny phosphors convert blue light from a standard gallium nitride light-emitting diode into different wavelengths based upon their size. Larger dots emit longer wavelengths (red), while smaller dots emit shorter wavelengths (green). This material is a precursor material to the next step in making our QD in aminiosilicone which is then blending together a mix of dot colors allows Nanosys to engineer a new spectrum of light. This allows liquid crystal display manufacturers to accurately match their light-emitting diode backlight to their light crystal display color filters to achieve the best possible color and efficiency performance. The result is professional photo and cinema level color performance in handheld devices, monitors, televisions, etc.

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## X

60 6 800 

## 1

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## X Nanosys, Inc 233 S Hillview Dr Milpitas Santa Clara CA 95035

Page 12 SANITIZED SUBMISSIONPage 13 SANITIZED SUBMISSIONGEN II QD Growth Process All Steps Sanitized Page 9 Att (EPA Submittal) 20140520 Rev 3.pdf

XXX XXX XXX 6 1 255 

### X X LS-S7	After addition and temperature ramp, hold at 210-220°C for 10-12 min, cool to 50-70 C XXX XXX 6 .5 255 

### X See continuation page. id: <P9SA2(1)C1R3> XXX XXX 6 .5 255 

### X See continuation page. id: <P9SA2(1)C1R4> XXX XXX 6 1 255 

### X See continuation page. id: <P9SA2(1)C1R5> XXX XXX 2 .3 255 

### X LS-S11	Add 66.5 mL of Growth Solution to a 250 mL centrifuge tube bottle. XXX XXX 3 4 255 

### X XXX XXX XXX 3 4 255 

### X X See continuation page. id: <P9SA2(1)C1R8> XXX XXX 3 4 255 

### X See continuation page. id: <P9SA2(1)C1R9> XXX XXX 3 4 255 

### X XXX XXX XXX 3 4 255 

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## (1)

See continuation page. id: <P9SA2(1)C1R11> XXX XXX 3 1 255 

### X See continuation page. id: <P9SA2(1)C1R12> See continuation page. id: <P9SA2(3)C1R12> 0.01% of residual quantum dots 3 0.5 255 See continuation page. id: <P9SA2(1)C1R13> See continuation page. id: <P9SA2(3)C1R13> 0.01% of residual quantum dots 3 .1 255 XXX XXX XXX 1 0.25 255 

### X X XXX XXX XXX 1 .25 255 

### X X XXX XXX XXX 1 .25 255 

### X X See continuation page. id: <P9SA2(1)C1R17> XXX XXX 1 .25 255 

### X GEN II S10	All tanks and lines are cleaned with a clean in place system using Toluene at 50 C. See continuation page. id: <P9SA2(3)C1R18> 0.01% of residual quantum dots 1 .25 255 See continuation page. id: <P9SA2(1)C1R19> See continuation page. id: <P9SA2(3)C1R19> 0.01% of residual quantum dots 1 .25 255

Page 15 SANITIZED SUBMISSIONP9SA2(1)C1R3 Part II, Section A, 2.(1) Worker Activity, Row 3

LS-S8	Replace thermocouple and septa cap with secured glass stoppers. Bring flask into the glove-box under vacuum using secondary containment, zip bag over the top and a cart

Page 16 SANITIZED SUBMISSIONP9SA2(1)C1R4 Part II, Section A, 2.(1) Worker Activity, Row 4

LS-S9	Move flask to glove box in a Ziploc bag and secondary container. Pour 370-590 g of shell solution into 1 L amber bottles and add 150-370 g of Toluene.

Page 17 SANITIZED SUBMISSIONP9SA2(1)C1R5 Part II, Section A, 2.(1) Worker Activity, Row 5

LS-S10	Quality Control -- Collect 14-16 mL in sealed cuvette. Determine Quantum Yield, wavelength, and Full Width Half Max (FWHM). Once analysis is complete liquid is discarded into solvent waste.

Page 18 SANITIZED SUBMISSIONP9SA2(1)C1R8 Part II, Section A, 2.(1) Worker Activity, Row 8

LS-S13	Remove from glove-box in bottles, shake vigorously for 30sec and centrifuge for 15min at 4000 RPM

Page 19 SANITIZED SUBMISSIONP9SA2(1)C1R9 Part II, Section A, 2.(1) Worker Activity, Row 9

LS-S14	Bring back into glove-box in bottles and pour off supernatant. Dissolve the precipitates in 13 mL of Toluene and combine into single container. Rinse bottles with remaining toluene.

Page 20 SANITIZED SUBMISSIONP9SA2(1)C1R11 Part II, Section A, 2.(1) Worker Activity, Row 11

LS-S16	Quality Control --Dilute 20μL of this solution in 4 mL of hexane. Filter and determine the optical density using the UV/vis spectrometer. Material is placed into cuvette in preparation for removal from glove box. Once analysis is complete liquid is discarded into solvent waste.

Page 21 SANITIZED SUBMISSIONP9SA2(1)C1R12 Part II, Section A, 2.(1) Worker Activity, Row 12

LS-S17	Laboratory glassware is placed into a 30% Potassium Hydroxide (KOH) / 70% Isopropyl Alcohol (IPA) base bath for a minimum of thirty minutes.

Page 22 SANITIZED SUBMISSIONP9SA2(3)C1R12 Part II, Section A, 2.(3) Prot. Equipment, etc., Row 12

Splash protection including gloves (PVC/Butyl/Neoprene outer gloves in combination with inner nitrile gloves), safety glasses, splash shield, lab coat and splash apron.

Page 23 SANITIZED SUBMISSIONP9SA2(1)C1R13 Part II, Section A, 2.(1) Worker Activity, Row 13

LS-S18	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).

Page 24 SANITIZED SUBMISSIONP9SA2(3)C1R13 Part II, Section A, 2.(3) Prot. Equipment, etc., Row 13

Splash protection including gloves (PVC/Butyl/Neoprene outer gloves in combination with inner nitrile gloves), safety glasses, splash shield, lab coat and splash apron.

Page 25 SANITIZED SUBMISSIONP9SA2(1)C1R17 Part II, Section A, 2.(1) Worker Activity, Row 17

GEN II S9	Quality Control --Dilute 20μL of this solution in 4 mL of hexane. Filter and determine the optical density using the UV/vis spectrometer. Material is placed into cuvette in preparation for removal from glove box. Once analysis is complete liquid is discarded into solvent waste.

Page 26 SANITIZED SUBMISSIONP9SA2(3)C1R18 Part II, Section A, 2.(3) Prot. Equipment, etc., Row 18

This is a closed system and personnel where lab coat, gloves, safety glasses, and face shield with connecting and discounting lines

Page 27 SANITIZED SUBMISSIONP9SA2(1)C1R19 Part II, Section A, 2.(1) Worker Activity, Row 19

GEN II S11	All Transfer tanks and flexible lines are taking to the stationary pumped cleaning system using Toluene.

Page 28 SANITIZED SUBMISSIONP9SA2(3)C1R19 Part II, Section A, 2.(3) Prot. Equipment, etc., Row 19

This is a closed system and personnel where lab coat, gloves, safety glasses, and face shield with connecting and discounting lines

Page 29 SANITIZED SUBMISSIONGEN II QD Growth Process All Steps Sanitized Page 9 Att (EPA Submittal) 20140520 Rev 3.pdf

LS-S8 0 0.005 kg/batch Off-site Incineration QD containated solvent and wipes are sent to a permited HW incinerator for disposal. 0 LS-S9 0 0.005 kg/batch Off-site Incineration QD containated solvent and wipes are sent to a permited HW incinerator for disposal. 0 GEN II S10 0 0.1 kg/batch Off-site Incineration See continuation page. id: <P9ASA3(5a)C1R3> 0 GEN II S11 0 0.01 kg/batch Off-site Incineration See continuation page. id: <P9ASA3(5a)C1R4> 0 GEN II S9 0 0.005 kg/batch Off-site Incineration See continuation page. id: <P9ASA3(5a)C1R5> 0 LS-S10 0 0.005 kg/batch Off-site Incineration See continuation page. id: <P9ASA3(5a)C1R6> 0 LS-S16 0 0.005Kg/ba tch Off-site Incineration See continuation page. id: <P9ASA3(5a)C1R7> 0 LS-S17 0 0.01Kg/bat ch Off-site Incineration QD containated solvent and wipes are sent to a permited HW incinerator for disposal. 0 LS-s18 0 0.01Kg/bat ch Off-site Incineration QD containated solvent and wipes are sent to a permited HW incinerator for disposal. 0

Page 30 SANITIZED SUBMISSIONP9ASA3(5a)C1R3 Part II, Section A, B.(5a) Control Technology & Efficiency, Row 3

Solvent from CIP contamined with QD in Aminosilicone and wipes are sent to a permited HW incinerator for disposal.

Page 31 SANITIZED SUBMISSIONP9ASA3(5a)C1R4 Part II, Section A, B.(5a) Control Technology & Efficiency, Row 4

Solvent from transfer tank/hose cleaning contamined with QD in Aminosilicone and wipes are sent to a permited HW incinerator for disposal.

Page 32 SANITIZED SUBMISSIONP9ASA3(5a)C1R5 Part II, Section A, B.(5a) Control Technology & Efficiency, Row 5

Waste samples contamined with QD in Aminosilicone and wipes are sent to a permited HW incinerator for disposal.

Page 33 SANITIZED SUBMISSIONP9ASA3(5a)C1R6 Part II, Section A, B.(5a) Control Technology & Efficiency, Row 6

Waste samples contamined with QD and wipes are sent to a permited HW incinerator for disposal.

Page 34 SANITIZED SUBMISSIONP9ASA3(5a)C1R7 Part II, Section A, B.(5a) Control Technology & Efficiency, Row 7

Waste samples contamined with QD in Aminosilicone and wipes are sent to a permited HW incinerator for disposal.

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Page 36 SANITIZED SUBMISSIONPage 37 SANITIZED SUBMISSIONPage 38 SANITIZED SUBMISSION001 Sanitized Process Steps Worker Exposure GEN II QD Growth Process All Steps Sanitized Page 9 Att (EPA Pt.2, Sec.A, End 3 002 Sanitized LOREX Requested Test Data PMN Testing Followup_UpdatedSanitized.pdf 5 004 Santized IES Order Results CAS_Page Intentionally Blank.pdf Pt.I, Sec.B, 1c. 2 005 Sanitized SDS GEN II - QD Growth Solution (Shell) SDS - Blank.pdf 13 008 Thermogravimetric Analysis Data Appendix B TGA Data.doc Worksheet: Other Property (Thermogravimetric Analysis ) 1 010 Sanitized Chemical Structure Diagram Chemical Structure Diagram - GEN II QD Shell - Blank.pdf Pt.I, Sec.B, 1e. 1

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## X Measured 0.996-0.897 Measured 999 Measured 20 Hexane <1 Measured 20

2.75-9 Measured 200 - 1000 cSt Measured Viscosity Page 40 SANITIZED SUBMISSIONTypical Concentration "Cd 9100 ppm Se 1700ppm Zn 14500 ppm S not reported" Measured Thermogravimetric Analysis 

## X 008 85-95 % Voliatle at 600 C Measured Solulbility Ethanol 20C 999 g/l Measured

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## ATTACHMENT HEADER SHEET Attachment Number 001 Attachment Name Sanitized Process Steps Worker Exposure 

## Associated PMN Section Number

Pt.2, Sec.A, End Does not contain CBI 

## Report Number NANO141022147946419

## ATTACHMENT HEADER SHEET Attachment Number 002 Attachment Name Sanitized LOREX Requested Test Data 

## Associated PMN Section Number

N/A Does not contain CBI 

## Report Number NANO141022147946419

## ATTACHMENT HEADER SHEET Attachment Number 004 Attachment Name Santized IES Order Results 

## Associated PMN Section Number

Pt.I, Sec.B, 1c. Does not contain CBI 

## Report Number NANO141022147946419

## ATTACHMENT HEADER SHEET Attachment Number 005 Attachment Name Sanitized SDS 

## Associated PMN Section Number

N/A Does not contain CBI 

## Report Number NANO141022147946419

## ATTACHMENT HEADER SHEET Attachment Number 008 Attachment Name Thermogravimetric Analysis Data 

## Associated PMN Section Number Worksheet: Other Property (Thermogravimetric Analysis )

Does not contain CBI 

## Report Number NANO141022147946419

## ATTACHMENT HEADER SHEET Attachment Number 010 Attachment Name Sanitized Chemical Structure Diagram 

## Associated PMN Section Number

Pt.I, Sec.B, 1e. Does not contain CBI 

## Report Number NANO141022147946419