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Supplementary Material for: Pneumatically Modulated Liquid Delivery with Feedback Control Electronics Table S-1: A summary of the Arduino Uno microcontroller pin connections to each component in the PMLDS. Arduino Uno Pin Reset 3.3V 5V Function Not connected Not connected Power supply GND Ground GND Vin A0 A1 A2 A3 A4 A5 D0 D1 D2 D3 D4 D5 D6 D7 D8 D9 D10 D11 D12 D13 GND AREF Ground 9V input Not connected Not connected Not connected Not connected SDA SCL TTL RX TTL TX LCD LCD LCD LCD LCD LCD 10’s switch 10’s switch 1’s switch 1’s switch Not connected Not connected Not connected Not connected Component Pin LCD Pin 2, LCD Pin 15, 1’s increment, 1’s decrement, 10’s increment, 10’s decrement, MAX517 Pin 6, MAX517 Pin 7, MAX517 Pin 8, MAX232 Pin 16 LCD Pin 1, LCD Pin 3, LCD Pin 5, LCD Pin 16, MAX517 Pin 2, MAX517 Pin 5, MAX232 PIN 15 Voltage regulator Voltage regulator MAX517 Pin 4 MAX517 Pin 3 MAX232 Pin 12 MAX232 Pin 11 LCD Pin 14 LCD Pin 13 LCD Pin 12 LCD Pin 11 LCD Pin 6 LCD Pin 4 10’s increment 10’s decrement 1’s increment 1’s decrement Figure S-1: The electrical diagram with the microcontroller and EPC housed in a single 3x4x5 inch aluminum box with a 24 V, 0.9 A power supply and a voltage regulator. Pressure Vessels Five pressure vessels were considered for use with the PMDLS. A 50 mL Nalgene centrifuge tube was tested, but based on documentation it could not hold 50 PSIG of pressure. Theoretically, the EPC unit is supplied with house air, which is down regulated to 50 PSIG. If the EPC unit were to fail, 50 PSIG could be supplied to the pressure vessel, while only a maximum of 15 PSIG is supplied when the EPC unit is in use. A pressure vessel capable of at least 50 PSIG was desirable for safety considerations, and necessary if higher flows and pressures were needed in future applications. A 500 mL Nalgene bottle was also considered, but a noticeable deformation was observed under 15 PSIG of pressure. A glass, 350 mL round bottom flask was found capable of holding 150 PSIG (Chemglass Scientific Equipment, Inc.). The glass round bottom flask had adequate volume to run continuously for several days at 30 μL min-1 and a visible indication of liquid level in the vessel. An inert plastic “T” connector (P-714, IDEX Health & Science) was used to connect the liquid flow and pressure line to the cap provided with the round bottom flask. The plastic cap was drilled and tapped for an adaptor (U-511, IDEX Health & Science) to connect to the “T.” Plastic capillary tubing (360 μm OD, 150 μm ID) was inserted through the “T” and into the round bottom flask for the liquid connection, while 1/16 inch OD thick-walled PTFE tubing was used for the gas connection. The completely assembled round bottom flask can be seen in Figure S2A. A metal, refillable spray paint canister rated for 100 PSIG was evaluated. The canister was modified slightly to hold 50 mL plastic centrifuge tubes and 1/16 inch OD PTFE tubing for liquid flow. The 50 mL centrifuge tube offers improved reusability of the pressure vessel without flushing or rinsing, minimizes cross contamination, and the same containers can be used for solution preparation. Figure S-2B shows the modified refillable spray paint canister with liquid and gas connections. Again, a complete parts list can be found in Appendix A. The metal canister is not transparent and the liquid level inside the 50 mL plastic centrifuge tubes cannot be monitored visually. With the exception of the 500 mL Nalgene bottle, the three other pressure vessels could be used depending on the application and experiment, but the glass round bottom flask and metal canister are better suited if a failure occurs and easily adapted for applications requiring higher pressures and flow rates. A custom built pressure vessel with designed to minimize dead volume and combine the advantages of the clear, round bottom flask with the refillable spray paint canister. Figure S-3 shows the custom pressure vessel used for collecting flow rate data to compare to the syringe pump. The pressure vessel is capable of holding 100 PSI of pressure and uses a snap tight lid, which acts as a failsafe for over pressure. The empty pressure vessel has a dead volume of approximately 90 mL, but the 50 mL centrifuge tubes occupy a approximately 75 mL when filled with 50 mL of liquid, resulting in a filled dead volume of 15 mL. Figure S-2: Pressure vessels for the PMLDS: (A) a 350 mL glass round bottom glass rated to 150 PSIG and (B) a refillable spray paint canister rated for 100 PSIG. An inert plastic “T” connection is used with the round bottom flask for fluidic and gas connections. PTFE capillary tubing (360 μm OD, 150 μm ID) was used as the liquid connection for the round bottom flask and thickwalled PTFE 1/16 inch OD tubing for the gas connections. The refillable spray paint canister used only thick-walled PTFE 1/16 inch OD tubing for both the liquid and gas connections. Figure S-3: A custom pressure vessel with a window for viewing the contents of the container during use. The empty pressure vessel has a dead volume of approximately 90 mL and a filled dead volume of 15 mL Parts List Table S-2: The complete parts list for the PMDLS. Part Description 24V, 0.9A Power Supply Toggle switch Mom-Off-Mom Toggle switch On-Off DPST Header pins, 36 pos Terminal crimp connector Female spade crimp connectors Fork Tongue crimp connector 10K Ω Resistor 2K Ω Resistor 10 Ω Resistor 0.1 μF capacitor 1 μF capacitor RS232-to-TTL chip 1-CH 8-Bit I2C DAC Chip Microcontroller Qty 1 2 1 5 7 3 1 6 1 1 2 5 1 1 1 4P4C Modular Jack PC Mount 1 16-pin DIP Socket 1 8-pin DIP Socket 1 Power Connector Port 4 x 5 x 3 in Aluminum utility box DB9 Male connector White on Black LCD Display 1 1 2 1 2 8 2 2 4 8 8 8 7 1 2 2 1 1 4 1 6 channel 4'' jumper cable Nylon 1/8 inch spacers M2x4 screw M2x16 screw M2 nut M2 washer M3x10 screw M3 nut M3 washer, zinc M3 nylon washer 4-40 socket cap screw ¼ inch 4-40 metal washer 4-Pin KK Connector (0.156’’ pitch) 3-Pin KK Connector (0.156’’ pitch) Connection terminal female 2-Pin housing with locking ramp Part Number ZPSA20-24 A105SYZQ04 M2021SS1W03 68001-436HLF 08-50-0107 19003-0107 31N2550 Manufacturer TDK-Lambda TE Connectivity NKK Switches FCI Molex Molex Newark Electronics CFR-25JB-10K MFR-25FBF-2K10 CFR-25JB-10R C315C104M5U5TA Yageo Yageo Yageo Kemet FK24Y5V1H105Z MAX232CPE+ MAX517BCPA+ Uno TDK Corporation Maxim Maxim Arduino TM3RA-44(50) 1-390261-4 1-390261-2 Hirose Electric Co Ltd TE Connectivity TE Connectivity JR-101 AU-1028 G17S0910110EU LCD-00709 Multicomp Bud Industries Amphenol Sparkfun Sparkfun McMaster-Carr McMaster-Carr McMaster-Carr McMaster-Carr McMaster-Carr McMaster-Carr McMaster-Carr McMaster-Carr McMaster-Carr McMaster-Carr McMaster-Carr PRT-10366 94639A299 92005A033 92005A037 90591A111 91166A180 92005A120 90591A121 91166A210 95610A130 92949A106 94744A155 09-50-3041 09-50-3031 08-52-0072 22-01-3027 Molex Molex Molex Molex 3-Pin housing with locking ramp 4-Pin housing with locking ramp Connection terminal female 2-Pin header with friction lock 3-Pin header with friction lock 4-Pin header with friction lock 4 1 18 1 4 1 22-01-3037 22-01-3047 08-50-0114 22-27-2021 22-27-2031 22-27-2041 Molex Molex Molex Molex Molex Molex Jumper shorting connector 2 STC02SYAN Sullins Connector Solutions 1 SS-400-1-2 Swagelok 1 SS-100-1-2BT Swagelok 1 SS-200-61-1 Swagelok 2 96371A203 McMaster-Carr 1 92141A029 McMaster-Carr 1 91525A230 McMaster-Carr 1 5 ft 5 ft 5 ft 5 ft 1 2 1 1 U-511 1503 1478 1932 1933 F-185x P-440 F-331x 11181 1 CG-1880-42 IDEX Health & Science IDEX Health & Science IDEX Health & Science IDEX Health & Science IDEX Health & Science IDEX Health & Science IDEX Health & Science IDEX Health & Science Eastwood Chemglass Scientific Equipment 1/8 inch NPT male to 1/16 inch Swagelok Male stainless steel 1/8 inch Swagelok male to 1/8 inch NPT female bulkhead stainless steel 1/8 inch Swagelok male to 1/16 inch Swagelok male bulkhead stainless steel 5/16 inch ID PTFE washer 5/16 inch ID, 5/8 inch OD stainless steel washer Large fender washer, 1.25 inch OD, 5/16 inch inner 1/8 inch NPT to ¼-28 Male 1/16’’ OD, 0.030’’ ID PTFE tubing 1/16’’ OD, 0.008’’ ID PTFE tubing 360 μm OD, 100 μm ID HPFA tubing 360 μm OD, 150 μm ID PTFE tubing 360 μm ID capillary sleeves 10-32 coned Bulkhead Union 10-32 PEEK Nut and Ferrules Billet refillable spray paint can 350 mL glass round bottom flask RS-232 Communication with a computer As of version 2.0.0, the NRL-PMLDS software and hardware is capable of communicating with a computer, or similar device, via the RS-232 protocol. A standard D-sub miniature 9-pin connector (DB9) is mounted on the back of the NRL-PMLDS with the following pin configuration for serial communication: Table S-3: Pin configuration for the DB9 connector Pin 1 2 3 4 5 6 7 8 9 Function Not connected TX RX Not connected Ground Not connected Not connected Not connected Not connected The NRL-PMLDS can be connected to a computer with a standard DB9 serial cable. A null modem, or crossover, cable is not necessary. A Serial-to-USB adaptor can also be used to enable USB communication with a computer but USB is not natively supported within the NRLPMLDS system as of version 2.0.0. The flow rate selector switches can be used to set the target flow rate while the NRL-PMLDS is in serial communication with a computer, or similar RS-232 enabled device. Serial communication offers greater control and functionality over the simple PID control and target flow rate selection interface. The NRL-PMLDS communicates via the RS-232 protocol at 9600 baud rate, 8 bits, 1 stop bit, no parity, and no hardware flow control. All commands must be terminated with a new line character (“\n”) and all responses from the NRL-PMLDS are terminated with a new line character. Table 2 outlines the commands recognized by the NRL-PMLDS. All other commands are ignored and any additional characters after the command are ignored. The number sign (“#”) in the commands are replaced with digits from 0-9 and are simply placeholders for the value. Floating point numbers can be sent as decimals or in scientific notation. Commands are not echoed back. The commands DF=##.#, KP=#.##E#, KI=#.##E#, and KD=#.##E# can only be set, or written, up to a combined total of 100,00 cycles. These values are stored in the internal EEPROM of the microcontroller and have a finite number of write operations. Use caution to minimize excessive calls to these commands. It is also recommended to send the restart command (“|>”) after setting the PID parameters. Table S-4: Summary of commands recognized by the NRL-PMLDS using a 9600 baud rate, 8 bits, 1 stop bit, no parity, and no hardware flow control. All commands must be terminated with a new line character (“\n”) and all responses are terminated by a new line character. Command TF=##.# TF? DF=##.# DF? AF? IF? V=#.## V? P=##.# P? KP=#.##E# KP? KI=#.##E# KI? KD=#.##E# KD? || |> Description Sets the target flow rate in μL/min, range: 10-99 μL/min, values greater than or less than the acceptable range are set to 99 and 10 μL/min, respectively. Gets the target flow rate in μL/min Set the default flow rate in μL/min, range: 10-99 μL/min, values greater than or less than the acceptable range are set to 99 and 10 μL/min, respectively. The default flow rate is the target flow rate on power up. This value is retained during power cycling. Gets the default flow rate in μL/min. This value is retained during power cycling. Gets the average flow rate in μL/min, flow rates greater than 100 μL/min are reported as 100 μL/min. The average flow rate is a 10-point, non-zero rolling average to reduce the noisy measurements from the flow meter. Gets the instant flow rate in μL/min, which is not part of the 10-point, non-zero rolling average. Sets the EPC control voltage in volts, range: 0-5 V, values greater than or less than the acceptable range are set to 5 and 0 V, respectively. Values must be left and right padded with zeros to match the proper length. The PID control must be paused (“||” command) to set the control voltage. Gets the EPC control voltage in volts. Sets the pressure in PSI, range: 0-15 PSI, values greater than or less than the acceptable range are set to 15 and 0 PSI, respectively. Values must be left and right padded with zeros to match the proper length. The PID control must be paused (“||” command) to set the pressure. Gets the pressure in PSI. Sets the Kp constant for the PID control. This value is retained during power cycling. This value is unitless and does not have to be in scientific notation. Gets the Kp constant for the PID control. This value is retained during power cycling. This value is unitless. Sets the Kp constant for the PID control. This value is retained during power cycling. This value is unitless and does not have to be in scientific notation. Gets the Kp constant for the PID control. This value is retained during power cycling. This value is unitless. Sets the Kp constant for the PID control. This value is retained during power cycling. This value is unitless and does not have to be in scientific notation. Gets the Kp constant for the PID control. This value is retained during power cycling. This value is unitless. Pauses PID control. The screen will replace “TF: ##.#” with “Paused”. In pause mode, the control voltage and/or pressure can be set manually. Resumes PID control. The screen will display the target flow in μL/min. The control voltage and/or pressure cannot be set manually while PID control is active