To: Adam Hall <a.hall@northeastern.

edu>
From: Sanjana Phatak phatak.s@husky.neu.edu
Date: 22 May 2017
Subject: Updated DART Q-TOF MS Guide

Dear Dr. Hall,

I am writing to present an updated instructional document I have created, for the
operation of the DART Q-TOF MS instrument.

The document used for my training was outdated and somewhat unclear, so I have started
from scratch to create this new guide, instead of using the previous document as a template. The
document I have produced aims to clearly explain the steps required for the efficient and
accurate operation of the instrument, providing a procedure with text and visual aids.

During my training with you, I noticed that a large amount of your personal time was Commented [E1]:
spent training me. My hope is that this new instructional document will be comprehensive Commented [E2R1]: Consider During my training with
enough that it shortens the amount of time spent educating new trainees, and serves as a you at [institutions name here], I noticed that.
reference for those who are already comfortable operating the DART Q-TOF MS.

I have been your student since May 2016 and have worked under you at the Barnett
Institute since January 2017, so you have been able to observe my dedication and work ethic in Commented [E3]: You mention the institute name here,
various environments. I have completed two co-ops and two courses specifically dedicated to but I think the letter could be improved if you establish the
institution earlier.
analytical chemistry, where I learned about and operated various analytical instruments. Also,
you yourself spent two months teaching me all I know about the DART Q-TOF MS instrument,
so I hope that you trust the validity of this document.

At your own convenience, please take the time to review the document, which I have
attached to this email. Please inform me of any edits or revisions, so that it can be put into use as
soon as possible.

You may contact me at phatak.s@husky.neu.edu or at 609-529-7447, and I will make

myself available to discuss the document in person or over email.

Thank you for considering my request, and for taking the time to provide feedback. I am
looking forward to the implementation of the updated instructional document.

Respectfully yours,

Sanjana Phatak
Research Assistant

Attached: DART-MS Guide.doc

DART Q-TOF MS: A guide to high throughput analysis by Direct Analysis in Real Time (DART) Commented [E4]: Not sure this acronym is necessary, since
it is included in DART Q-TOF MS.
Quadrupole-Time of Flight Mass Spectrometry

Setting up the DART Ionization Source: Commented [E5]: Before you go straight into the
procedure, I think it would be helpful to have an
1) Open the helium valve to 80 psi, such that the lever is in line with the meter and tubing. The helium introductory paragraph that orients the reader. It would be
helpful to know the general information of the procedure:
valve is the 3rd valve from the front in the top row, and has tygon tubing, an orange press tight fitting, why you would use it, how long it takes, etc.
and the label HE.

2) Turn on the vacuum pump, which is located below the instrument on the same bench as the LC stack. Commented [E6]: Im glad to see you took so many
pictures. I wouldnt know what a vacuum pump looks like.
3) Turn on the power to the DART ionization source controller, which is the blue box above the
instrument.

4) Open the DART software window on the computer. Enter 192.168.10.111 if it is not already present.
a. Click standby, then set the appropriate starting temperature to commence heating. Commented [E7]: What is the appropriate starting
temperature? How will we know?
b. Open the methods tab, located on the bottom left. One of the following options may be
chosen:
i. Quickstrip Temperature Profiles: Choose edit, and input the information required for Commented [E8]: I feel slightly disoriented with 4a and 4b
on separate pages, and 4b being so long. It would probably
the sample. The heater wait time is always 1 second and the contact closure delay is be best to make 4b a whole new step: step 5
always 5 seconds. The sample speed will be between 0.5 mm/sec and 1.0 mm/sec. Once
the settings have been configured, click save changes.
ii. Quickstrip: All of the settings will be the same as for the Temperature Profiles method,
but the temperature increment parameter will not be an option
Setting up the Q-TOF Mass Spectrometer:
1) Right click on the MS Q-TOF icon and click standby to put the MS into standby mode. Commented [E9]: I love how each step has a clear
objective, highlighted in the picture. Good work drawing the
readers attention with red boxes/arrows

2) Sample: In the sample tab, change the sample name and data file name as necessary (i.e. 170501 for
May 1, 2017). The data file name should be the same as the sample name, but with a .d after the
name. Keep the run type manual start, and check to ensure the pathway goes to the correct folder
within the MassHunter Software. The folder can be changed by clicking the three dots after the path.

3) Properties: In the properties tab, change the path and description if necessary. The path should be the
appropriate method, and the description is optional but may be used to differentiate between similar
samples.
4) MS Q-TOF:
a. General tab: Do not change any default settings other than choosing an appropriate stop time.
Start with a stop time that is longer than necessary, based on the sample speed.

b. Acquisition tab: Set an appropriate mass range. Start with 50-1000 m/z, unless the target mass
range is already known. If this is the case, narrow the mass range to increase sensitivity.

c. Chromatogram tab: Input an EIC range if an extracted mass range is desired. Otherwise, keep it
the same as the TIC range.

Commented [E10]: Good job keeping the entire step 4 on

this one page
d. Keep the Source and the Ref Mass tabs at their default settings. Commented [E11]: Definitely include page numbers.
Theyll be of tremendous help if this document is ever
printed.
Analysis of samples by DART Q-TOF MS:
1) Right click on the MS Q-TOF icon to turn the MS on. Let it run for a couple of minutes prior to sampling.

2) Leave at least one sample spot blank on the Quickstrip for the collection of background data. Ideally,
this should be the first or the last spot.
3) For a temperature profile run, spot the appropriate volume onto each mesh sample region, leaving
every third sample spot blank. This volume is typically between 2 and 5 L.

4) Allow the Quickstrip to dry until the spots are not visible. This takes a few minutes depending upon the
solvent high volatility solvents such as acetone, methanol, ethanol and isopropanol are desirable.
5) Place the Quickstrip card into the linear rail with sample 1 on the left and sample 12 on the right.
6) Click the start sample run icon in the top panel of the Agilent MassHunter software.

7) Once the MS Q-TOF icon and the icon under instrument status (on the top right) turn blue and the
software says run, click start in the DART software window.

8) Click the view data button in the software to analyze data once the analysis run is complete.
Alternatively, double click the Qualitative Analysis icon on the desktop.
a. Click and drag the cursor across the x-axis of one peak, then double click on the selected peak
to generate the MS data for that peak.
Shutdown Procedure for the DART Q-TOF MS System:
1) Put the MS into standby mode by right clicking the MS Q-TOF icon window. Put the DART into standby
mode and lower the heater temperature to 150 degrees, or turn it off completely.

2) Once the source temperature lowers to 150, turn the DART controller and the vacuum pump off.

3) Finally, shut off the helium valve for the DART ionization gas. Commented [E12]: Consider including a closing sentence
or two about the completion of the procedure and what
comes next.
Dear Sanjana,

Great work on this guide. It was very thorough with the tons of pictures included, and I think that if I
was placed in your lab, I could conduct this procedure. This is mostly due to the fact that instruments that
could be completely unknown to the reader are shown for verification. This also serves to comfort the reader
while he/she is completing the procedure.

The nature of a guide with as many pictures as yours calls for a difficult time formatting. It is important
to pay close attention to the page breaks and see what steps you are separating in each subsection. I have
highlighted some examples that can be improved in my margin comments.

I also suggest that you include some short sentences to orient the reader. These sentences will serve to
declare a purpose for the procedure instead of being thrown straight into it. These comments should be left in
the very beginning of the procedure and at the very end.

Your cover letter was also very well executed overall. It highlighted a problem, and brought the
readers attention to fix that problem. You have included all of the suggested information from Prof. Akbari in
your cover letter, which makes for a full immersion into the context.

Well Done,

Eric