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Tampa Bay Buccaneers
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Absolute horseshit
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This game is embarrassing. We look completely horrible on both sides of the ball. It's completely unacceptable. Jamies is throwing with absolutely no accuracy and they game up on the run on the first drive. They better be ready to play in the 2nd half. Personally, I don't see it happening
Marpet is snapping the ball terribly, the guy was a borderline All-Pro guard but let's **** with his development. Maybe he can play OT next year
Finally into the end zone now let's see if our defense can stop their 2nd string QB
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Our entire defense needs to get out 9n the bench. They are absolutely terrible
Thanks for throwing the game away Jameis. Worst game he has played since year 1
And im the one whose negative in this forum and bringing down the morale ^^^^^ lol. Ya i think we will be 9 and 1 this games easy no Bradford. Giants are garbage. Win here win there. Eat your words. Keenum is 3 and 0 now against us. Giants look much better. We have tonnes of injuries on defence now. Everything i said would happen did. Bad karma.
Last edited by BucsFan47; 09-24-2017 at 03:56 PM.
^Bucs lost because of the things we said. You are really a ****ing joke man. Please find another forum. You could not be more unwanted in here
You guys said we would be 9 and 1 and we should win this game because of no bradford? I told u guys to stfu bc in professional sports u do not look ahead and project wins bc it will come back on you and its bad karma. If you think you are right you must be missing some chromosomes. And unwanted? Am i supposed to be upset? This is a forum.... nobody in here are friends. Its an internet forum lol. I could care less if u feel im unwanted. Im laughing out loud at you right now. I was right. You dont overlook teams and players in professional sports. I know first hand. You probably have sat on your couch for your whole life eating potato chips. 1 and 1 bc of your bad karma. Smh at you!
How was theWinston interception when he was throwing to Evans in the end zone not called pass interference? Or hitting a defenseless receiver? He went high on Evans and hit him up around the head?
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Big changes in the air, can't you just feel it? The Vineyard Haven Public Library welcomes all from 11:30 a.m. on Tuesday to watch, hope, cheer on, and enjoy the inaugural day proceedings in their community room. I am hoping to be done with my dentist appointment in time to join you there.
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Action, romance, and comedy? No kidding. Get down to the Katharine Cornell Theatre tonight by 7:30 p.m. for a most unusual 2006 German film, The Kebab Connection. The plot is too twisted, strange and hilarious to describe in detail here. Just go.
A more serious subject is the weather and our preparedness for ice storms and other natural disasters. American Red Cross volunteers Ted Smith and Glen Beasley will be interviewed about our area's plans. They will speak on volunteering as well. You may catch three times for the program on radio Sunday, Jan. 18. Airings will be at 6 a.m. on WFCC 107.5, at 7 a.m. on WQRC 99.9, and at 8 a.m. on Ocean 104.7. For more information contact Cape and Islands Red Cross at firstname.lastname@example.com. Stay informed, stay ready, volunteer.
I have been blessed to have such fabulous neighbors in my 'hood. Sadly, for all of us, neighbor Jan Baclawski died at his Connecticut home on Jan. 3. Our condolences to his wife, Rosemary, and his large and extended family. Any of them I met here on Island were always so kind, polite and interested in their neighbors. Jan himself was such a gentleman; he will be greatly missed by us all.
The birthday bandwagon pulls along Maribeth Roden, Thaw Malin, Joaquim Balboa and Myra Romain today. Tomorrow belongs to Rosemary Gambino. Jan. 18 is shared by Anthony Cardoza and Ronnie Daw. On Jan. 19 Ciara Seccombe turns nine and celebrates that day with Patti Linn, Mandy King Rice, Ruth Major and Elizabeth Hume Hall. Jan. 20 is a party for the wondrous Patricia Neal, Kim Montanile and Mary-Beth Priore. Jan. 21 is for Carol Whitmarsh, Noah Casner, Annie McEvoy, Ned Hehre and Travis and Derek Fennell. And on Jan. 22 Donna Bouchard takes the cake. Many happy returns.


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Stories of restaurants transitioning to a no-tip policy have been slowly infiltrating the news for the past year. This change has been brought on for a variety of reasons: Minimum wage increases, simplified business reporting and employee satisfaction, to name just a few of the reasons for this transition.
A hot topic across all industries — especially the restaurant industry — is employees earning a livable wage. Several cities and states have taken it upon themselves to raise minimum wages from the federal mandate of $7.25 an hour for non-tipped employees and $2.13 an hour for tipped employees. For example, the City of Chicago recently mandated a minimum wage of $10.00 an hour for non-tipped employees and $5.45 an hour for tipped employees.
Some restaurants are transitioning to a no-tip platform to help respond to employee complaints regarding poor salaries. A no-tip platform provides a consistent paycheck for employees each week. In conjunction, many restaurants are implementing sales-based incentives and team goals for employees to ensure that service remains up to par. Employer benefits include simplified business reporting and tax compliance.
Transitioning to a no-tipping policy will likely require an increase in menu prices or a flat-rate service charge to recoup the lost tip income from customers. One thing to keep in mind if you are considering transitioning to a no-tip model is the IRS has ruled that automatic gratuities and service charges are distributed to employees as wages, not tips. This is an important distinction for tax reporting purposes, as it would exclude restaurants from claiming the FICA tip credit. On a side note, the Obama administration's FY 2016 Revenue Proposal would repeal the FICA tip credit as proponents of the repeal suggest the cost of the tip credit outweighs the positives of tax compliance.
There are many options to weigh when deciding if a no-tip model is suitable for your restaurant, employees and customers. An employer thinking of implementing a no-tip policy should discuss the possible change with your employees and advisors to verify it makes both social and economic sense. As the landscape changes, as a customer, be aware that your next meal out may include a service charge rather than a tip line on your check.
The content of this article is intended to provide a general guide to the subject matter. Specialist advice should be sought about your specific circumstances.


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The U.S. Senate Foreign Relations Committee is holding a hearing Tuesday on the president's authority to order a nuclear strike against another country.
The hearing comes as President Donald Trump continues to exchange insults with North Korean leader Kim Jong Un, who has overseen nuclear and missile development programs that have progressed faster than most global weapons experts anticipated.
For the first time in more than four decades, Congress will examine the president's authority to wage nuclear war. Existing procedures require the president to first consult with military and civilian leaders, but the final decision is made by the president.
Senator Bob Corker, arguably the most vocal Republican critic of Trump, will preside over the hearing. Corker said a number of lawmakers have raised questions about the process and deployment of the U.S. nuclear arsenal.
'This discussion is long overdue,' Corker said when he announced the hearing.
Two Democratic lawmakers, Representative Ted Lieu and Senator Ed Markey, each have submitted legislation that would prohibit the president from ordering a preemptive nuclear attack without a declaration of war by Congress. The measures, though, have not advanced in the Republican-controlled Congress.
Corker said in an interview with the New York Times the president's heated rhetoric toward North Korea could further escalate tensions that could lead to World War III, prompting some nuclear weapons experts to welcome the hearing.
Stevens Institute of Technology's Alex Wellerstein, who has researched extensively about presidential nuclear authority, said he hopes the hearing 'might shed some light on aspects of the procedures for presidential use of nuclear weapons that I think really needs to be known and talked about.'


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Lewis Hamilton qualified quickest for Sunday's French Grand Prix with the 75th pole position of his career, but said his Q3 was "so-so".
Ferrari's Sebastian Vettel leads Hamilton by one point at the top of the standings after seven of 21 races.
Daniel Ricciardo has moved up the rankings, with Bottas losing ground despite a good comeback drive after the early crash.
As the F1 Grand Prix Circus returns to France for the first time in a decade, it's Lewis Hamilton on pole after qualifying, alongside team mate Bottas. "But P3 I'm happy with because the vehicle should be good in the race".
"This place is lovely", he said.
Mercedes brought an upgraded power unit to Le Castellet and Hamilton, who has yet to win in France, has been consistently quick.
The Renault-powered Red Bulls were Mercedes' closest challengers as Ferrari languished nearly a second off the pace across both sessions.
"I hope that we can do something great with it".
Peru coach Ricardo Gareca may quit after World Cup exit
The team failed to find the net in their first two World Cup games againt Denmark and France , but Carrillo's strike made up for the goal drought, and is the country's first in World Cup competition since World Cup Spain 1982.
Bert van Marwijk feeling Australian ahead of facing 'emotional' Peru
It had been a long time before Peru had found the net in a World Cup. "I don't think you must force something from the beginning". It's a must-win game for the Socceroos, but a dead rubber for Peru who can not progress after 1-0 defeats to Denmark and France.
European Union supporters march in London to call for Brexit deal referendum
Meanwhile, Foreign Secretary Mr Johnson said people would not tolerate a " bog roll Brexit " that was "soft, yielding and seemingly infinitely long".
Charles Leclerc, 20, continued his impressive debut season by making the final shoot-out for the first time.
This was clear evidence not only of Hamilton s pure pace, but also his innate ability to learn a new circuit very quickly.
The 90-minute opening session was red-flagged with a minute remaining when Ericsson lost control at the Beausset corner, spun and hit the barriers hard, with the Sauber auto then catching fire.
Spain's double world champion Fernando Alonso, victor at the Le Mans 24 Hours with Toyota last weekend, came down to earth with a bump in 16th place with McLaren team mate Stoffel Vandoorne 19th.
"Our performance has usually been so-so on Saturdays, with our average position in qualifying so far this year being 13th", said Alonso.
"I'm really happy with the pole, but I always strive for perfection and there was some time left on the track, so I still have stuff to work on", he said.
McLaren still fared better than former champions Williams, who had Russian Sergey Sirotkin 19th and Canadian Lance Stroll 20th.
Kimi Raikkonen (Ferrari), Brendon Hartley (Toro Rosso), Esteban Ocon (Force India) and Vandoorne all spun onto the blue-striped run-off areas at Turn Six but stopped before hitting the barrier.
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Martinez not anxious despite ankle knock keeping Lukaku from trainingESPN's Nick Ames shares his thoughts on Belgium's dominant display against Tunisia which saw them top group G. Substitute Michy Batshuayi also got on the scoresheet, so Belgium have a class replacement ready to go.
James Harden is named 2017-2018 NBA MVPUnfortunately for him, his incredible playoff run didn't factor into the voting (since MVP is a regular-season award). Dwane Casey was crowned Coach of the Year after guiding the Toronto Raptors to first place in the Eastern Conference.
Looking up at the Night SkyThis full moon of the late June sky also has other names such as Honey Moon, Hot Moon, and Rose Moon. When is the Full Strawberry Moon? A plane flies in front of a full moon.
Alec Baldwin invites Melania Trump to 'SNL'Alec also shared a photo taken with Melania in 2007, writing, "We have a chair waiting for you in the @nbcsnl make-up room". In an apparent dig at Donald Trump , Baldwin said the show would welcome the First Lady "as a hero".
Expect A Cat-astrophic Win As Cat Predicts Nigeria's Victory Against ArgentinaArgentina go on to face Group C winners France on Saturday in the next round while Group D winners Croatia take on Denmark . I have not spoken to any of the Argentina players but I have heard the reports that the players wanted to get rid of him.
Fans, pundits react to Group B VAR chaosUruguay did not allow a goal in the group stage, and will be a risky team in the Round-of-16 match against Group B runner up. Russian Federation await Spain and the hosts will be tough opponents despite their 3-0 humbling at the hands of Uruguay.
Child Fired Loaded Gun He Found In A Couch At IKEAAuthorities said a child fired a shot inside an Indiana IKEA after finding a gun accidentally left on a couch by a customer. Ikea said in a statement it has a no weapons policy for its stores and that it was cooperating with police.
Iceland eliminated despite spirited display in loss to Croatia in RostovGylfi Sigurdsson levelled with a penalty but Ivan Perisic grabbed a last-gasp victor . A Nigeria win would send the Icelanders and Argentinians both home.
Woman Refused Pregnancy Termination Drugs at WalgreensArteaga opted to take the medical route, but the pharmacist she identified as Brian Hreniuc denied her the necessary prescription. How is this okay? "If you have gone thru a miscarriage you know the pain and emotional roller it can be", she wrote.
Trump threatens Harley-Davidson over European production moveIn addition to four US-based manufacturing facilities, Harley operates plants in Australia, India, Brazil, and Thailand. "Their employees and customers are already very angry at them", Trump said on Twitter, without providing any evidence.
Knoxville Nationals Winner Jason Johnson Passes Away Following Racing AccidentTony Stewart Racing posted: "While fierce competitors on-track, the racing family has a bond that's unbreakable". Per the Milwaukee Journal-Sentinel, Johnson was airlifted to a hospital after his crash.
Illness, injury could leave Sweden short against GermanyTunisia is in the World Cup for the first time since 2006 and had an admirable showing in its opener against England. It begins, however, with what should be a one sided Group G affair, as Belgium take on Tunisia.


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Post achievements to your institutional Facebook page and Twitter accounts using Social Media Connect. Social Media Connect can be found under Settings > Connections.
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Click the gear icon (settings) at the top of your Merit Dashboard
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Click "Sign in with Facebook." You must be signed in to the Facebook account which serves as an admin to your institution's page.
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Step 1 Click "Okay"
You will see your Facebook picture here. You will use your personal Facebook account to log in to Facebook as an Admin of your institution's Facebook fan page. Don't worry, Merit will only connect to the fan pages you're an Admin of.
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The final lightbox will ask you to allow for Facebook to "...manage your Pages and access your Facebook page and Apps insights." You will have to select Okay, you can not skip this step.
After clicking Okay, you will be redirected to Merit where you will find a notification that states you have successfully connected Merit to your institution's Facebook fan pages.
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Ion Mobility Spectrometry - High Resolution LTQ-Orbitrap Mass Spectrometry for Analysis of Homemade Explosives
- 609 Downloads
- Citations
The detailed chemical characterization of homemade explosives (HMEs) and other chemicals that can mimic or mask the presence of explosives is important for understanding and improving the performance of commercial instrumentation used for explosive detection. To that end, an atmospheric-pressure drift tube ion mobility spectrometry (IMS) instrument has been successfully coupled to a commercial tandem mass spectrometry (MS) system. The tandem MS system is comprised of a linear ion trap and a high resolution Orbitrap analyzer. This IMS-MS combination allows extensive characterization of threat chemical compounds, including HMEs, and complex real-world background chemicals that can interfere with detection. Here, the composition of ion species originating from a specific HME, erythritol tetranitrate, has been elucidated using accurate mass measurements, isotopic ratios, and tandem MS. Gated IMS-MS and high-resolution MS have been used to identify minor impurities that can be indicative of the HME source and/or synthesis route. Comparison between data obtained on the IMS/MS system and on commercial stand-alone IMS instruments used as explosive trace detectors (ETDs) has also been performed. Such analysis allows better signature assignments of threat compounds, modified detection algorithms, and improved overall ETD performance.
KeywordsHomemade explosive ETN Ion mobility Mass spectrometry ETD
On-line coupling between IMS and MS instruments has proven to be a powerful analytical platform with a multitude of successful applications from physics to biology [4, 8, 9, 10]. These include characterization of complex mixtures in proteomics and metabolomics, as well as 3-D structural elucidation of large biomolecules and their complexes [11, 12, 13, 14, 15, 16, 17, 18, 19, 20]. A number of IMS-MS studies aimed at elucidating various aspects regarding traditional IMS analysis of explosives and other threat compounds have also been reported [21, 22, 23, 24, 25, 26]. IMS can provide chemical separation based upon differences in the size, shape, and charge of analyte ions, and their effective interactions with drift gas molecules. In addition to IMS-derived information, MS can provide unequivocal identification of chemical species using high mass accuracy in combination with tandem MS. Drift-tube ion mobility (DTIMS) as well as differential ion mobility (DIMS) instruments have been interfaced with different types of mass analyzers (including time-of-flight, magnetic sector, and ion trap) resulting in powerful multidimensional analytical combinations [27]. Here we utilize a DTIMS instrument coupled to a tandem high-resolution/accurate mass (HRAM) MS instrument for characterization of threat materials. We illustrate the advantages of this system for characterization of gas-phase ion chemistry processes occurring during IMS analysis of explosives using ETN, synthesized from different starting materials and by different routes. In parallel, data have been acquired with a commercial stand-alone DTIMS-based explosives trace detection (ETD) system. The flexible atmospheric pressure IMS-MS interface readily allows for "gold standard" comparison with and characterization of current generation DTIMS-based ETD instruments, as well as future IMS threat detection systems that are in development. The IMS-MS instrument presented here is equipped with three different ionization sources – electrospray ionization (ESI), corona discharge (CD), as well as 63Ni. In addition, the IMS interface allows for modification of reagent/drift gases and the introduction of dopant materials, which can be used to alter the ionization chemistry or ion transport processes. Currently deployed ETD systems utilize 63Ni for ionization, whereas newer models rely on CD and other non-radioactive methods. Replacing ion sources in commercial ETDs may require alterations to the detection bands or algorithms used by these instruments. Therefore, a combined IMS-MS approach is also valuable to study the effects of alternate ionization sources on threat material identification. Although IMS combined with low resolution MS and MS/MS analyzers have been previously used to probe the gas phase ion chemistry of explosives [2, 21, 22, 23, 24, 28, 29], this is to our knowledge the first such study of explosives using a higher resolution DTIMS coupled to a high resolution MS/MS instrument.
Sample Preparation
Certified reference standard samples of explosives (PETN, ETN, TNT, RDX) were purchased from Accustandard (New Haven, CT, USA) as 1 mg/mL stock solutions in acetonitrile or methanol and were diluted as needed. In an effort to approximate clandestine preparation of explosives, small quantities of ETN were also synthesized in-house. Either food grade (Truvia brand sweetener, purchased from a local food store) or analytical grade erythritol were nitrated by reaction with acetyl nitrate or with mixed sulfuric and nitric acids, according to procedures detailed in Oxley et al. [30]. All required chemicals and solvents, including erythritol, acetyl nitrate, ammonium nitrate, sulfuric acid, isopropanol, and acetone, were purchased from Sigma Aldrich (St. Louis, MO, USA).
IMS, IMS-MS, and MS Analyses
For most experiments, explosive samples were ionized directly from solution by ESI operated at ~2.5 kV relative to the entrance of the IMS desolvation region. In some cases (specifically noted in the text), samples were first deposited on swabs (DSA Detection, North Andover, MA, USA) and then thermally desorbed at 180°C. Desorbed sample molecules (including products of thermal degradation) were ionized either by CD (operated at 1.8 kV in negative ion mode and 2.2 kV in positive ion mode; voltages relative to IMS desolvation region) or 63Ni. For all ionization sources, ions were sampled through an aperture into an intermediate desolvation/reaction region before injection through the entrance gate into the drift region (Figure 1). A cylinder of compressed, dry air (Ultra zero-grade; Airgas, Dallas, TX, USA) was used as an IMS drift gas, which was set to a flow rate of 2.5 L/min. (It is estimated that approximately 1.5 L/min of this gas flow is directly drawn into the mass spectrometer inlet, resulting in an effective drift gas flow of approximately 1 L/min.) In several experiments, approximately 1 ppmv dichloromethane was added directly to the drift gas using a temperature-controlled permeation tube heater (Excellims) to explore the effects of drift gas modifiers (dopants) on ion formation and ion transport processes. The temperatures of the ionization region, drift gas, and IMS housing were all adjusted to 150°C, which was found to be important for observation of stable chloride ion adducts with explosive standards such as PETN and RDX. Two Bradbury-Nielsen gates – entrance (BNG1, operated at 45 V relative to the drift tube) and exit (BNG2, operated at 150 V relative to the drift tube) – were used to inject ion packages into the 10.56 cm drift region and control the exit of separated ions, respectively. The gates were opened and closed by applying voltage across the wire electrodes with a typical gate pulse width of 70 μs. The drift tube was operated at 10 kV potential. BNG1 was at 62.94% and BNG2 at 7.67% of the total operating potential, resulting in 5.53 kV drop between the two gates (typical field strength of 525 V/cm). While these conditions were optimized for sensitivity and to achieve comparable results to the stand-alone ETD rather than high resolution, a resolving power of greater than 50 was readily achieved. Both positive and negative ion mode spectra were acquired, utilizing multiple detection modes for acquisition of IMS-MS data (see Discussion below). Measured drift times for unknown species were calibrated against well-characterized chemical standards (TNT and 2,6-di-tert-butylpyridine for negative and positive modes, respectively) in order to determine the respective reduced mobilities (K0) [32]. High-resolution MS-only data were also collected on the Orbitrap at better than 60,000 resolving power, allowing typical mass accuracy better than 3 ppm, following the manufacturer's standard external calibration procedure. Elemental composition assignments from the accurate mass data were determined using the calculators built into the Xcalibur software (Thermo Fisher Scientific). Two-dimensional (2-D) IMS-MS data analysis and plotting was performed using the Excellims developed software, VisIon Trap.
Stand-alone IMS data were collected using a Smiths Detection ETD (Ionscan 500DT; London, UK). This ETD instrument thermally desorbs samples from swabs for ionization in a 63Ni source and detects both positive and negative ions. All instrument parameters were under the control of the manufacturer software and could not be adjusted [33]. Instead, parameters for the hybrid IMS-MS system (e.g., desorber and drift tube temperatures) were adjusted as described above to allow observation of similar ion species in both systems for explosive standards such as RDX and PETN. A resolving power of ~40 has been reported for this standalone IMS instrument [29, 34]. Drift gas was supplied from room air that had been passed through a drying column to eliminate significant humidity effects. In some experiments, the manufacturer-supplied drift gas dopant cartridge that enhances explosive detection through formation of chloride adducts was removed to allow for direct comparison with the IMS-MS instrument. K0 values included in the manufacturer-supplied software package were cross-calibrated against published K0 values for well-characterized explosive standards.
Safety Precautions
Small-scale syntheses of energetic materials should only be conducted by appropriately trained personnel following all necessary safety protocols. Althugh solutions containing trace quantities of explosives are safe for manipulation and analysis outside of a fume hood, all such samples should be handled with caution. The radioactive 63Ni ionization source should be used only by appropriately trained personnel.
Results and Discussion
IMS-MS Coupling
We have utilized DTIMS-MS in parallel with traditional stand-alone ETD systems for characterization of threat materials. Typical drift times for a DTIMS are on the order of 10 ms. However, in order for a combined IMS-MS system to provide sufficiently resolved IMS data upon reconstruction, a mass spectrum must be acquired on the order of 10 to 100 μs. Such time scale "nesting" requirements typically restrict the type of mass analyzers that can be directly interfaced with DTIMS to time-of-flight (TOF) mass spectrometers. When IMS is combined with mass analyzers acquiring spectra on the order of hundreds of milliseconds, such as linear quadrupoles and ion traps, the combined system is generally operated in a low duty-cycle "scanning mode" (see below) in order to accommodate the disparate time scales. Several atmospheric pressure DTIMS combinations with ion trap mass analyzers, including an FTICR spectrometer, have been previously reported [10, 35, 36, 37, 38]. Recently, linear frequency chirping of the IMS beam and subsequent Fourier transform decoding of the MS signal has resulted in an increased overall duty cycle of the DTIMS-ion trap system [31]. This approach utilizes multiplexing schemes for ion beam modulation in the IMS including Fourier [39] and Hadamard [40] transforms, also utilized in hybrid DTIMS-TOF instruments [41, 42, 43].
The dual gate DTIMS-MS combination [35, 44] used here can operate in four distinct modes. In "open mode," ions drift continuously and unrestricted through both ion gates allowing conventional mass spectral data acquisition. Since ion signal is necessarily reduced in other IMS modes due to reduced duty cycle, high-resolution mass spectra on the Orbitrap are typically collected in "open mode." In addition, this mode facilitates adjustment and optimization of source operating parameters without removing the IMS. In "scan mode," the selected ion mobility range can be scanned by sequentially stepping the delay between the opening of the entrance and exits gates across the chosen range of drift times. This allows the generation of a comprehensive 2-D IMS-MS plot, which is of particular importance for the correlation of specific ion drift times with their corresponding mass spectra and for the multidimensional separation of components of complex mixtures. In "gated mode," mass spectra can be collected at individually specified ion mobilities by applying a predetermined delay between the opening of the entrance and exit gates respectively. This mode uniquely allows for the removal of contaminants and also targeted accumulation of ions in the trap for improved sensitivity and enhanced MSn fragmentation. Finally, the addition of a Faraday plate detector behind the IMS exit allows the DTIMS to function in "Faraday mode" as an independent, stand-alone instrument. This mode was used for comparison to the ETD system and for concurrent collection of full-scan IMS and MS data. Although the system is capable of operating in an "FT mode" [31], this mode was not utilized for these studies.
ETN Analysis by IMS-MS
Summary of Ion Species Observed in IMS-MS Analysis of ETN Using Different Ionization Modes. Chemical Formulas for Each Species were Confirmed Using Accurate Mass Measurements and Isotopic Distribution Patterns. MS/MS Fragments for ESI-Generated Species are Shown
Anion species
Elemental composition
Experimental accurate mass (Δ from calculated)
Ionization mode
MS/MS fragments (ESI only)
[ETN–NO2 + H + Cl]–[ETriN + Cl]–
C4H7N3O10 35Cl
291.9818 (3 ppm)
63Ni (with dopant)
[ETN + H]–[ETriN + NO2]–
303.0058 (3 ppm)
ESI, CD, 63Ni
241, 261, 259, 271, 285
[ETN + OH]–[ETN–NO2 + H + NO3]–[ETriN + NO3]–
319.0029 (4 ppm)
ESI, CD, 63Ni
125, 229, 255, 275, 301, 303
[ETriN + SO3-H]–
335.9635 (2 ppm)
139, 151, 164, 179, 227
[ETN + Cl]–
C4H6N4O12 35Cl
336.9660 (5 ppm)
63Ni (with dopant)
363.9857 (2 ppm)
ESI, CD, 63Ni
142, 255, 347
[ETriN + TFA-H]–
369.9994 (2 ppm)
ESI, CD, 63Ni
113 (112.9854)
[ETN + 2Cl]–
C4H6N4O12 35Cl2
371.9346 (5 ppm)
63Ni (with dopant)
Evidence for the possible presence of ETriN in solution is further provided by the observation of additional ion species during the IMS-MS analysis of ETN by CD or 63Ni ionization (Table 1). Analogous to m/z 319 species, the Cl adduct ion at m/z 292 can be a mixture of two ions having the same elemental composition, ETriN and a gas-phase ETN fragment, resulting from the loss of NO2 (as denoted in Table 1). While nominally the anion at m/z 303 is denoted as [ETN + H]–, ion formation by hydride addition to ETN seems much less likely compared with the formation of the [ETriN + NO2]– anion adduct with the same elemental composition. Moreover, based on accurate mass measurements, a species at m/z 370 can be interpreted only as an anion adduct of ETriN with trifluoroacetic acid (TFA), plausibly present as a trace impurity either during synthesis or analysis. Indeed, tandem MS data confirmed this assignment, where the sole strong fragment ion was found to have an elemental composition (C2F3O2) corresponding to [TFA – H]– (Table 1). No [ETN + TFA – H]– adduct was observed. Presumably TFA ion pairing occurs only with ETriN that contains a free hydroxyl group. The ETriN adduct species was observed to be present only in ETN samples synthesized in-house as well as in commercially produced ETN stored for an extended period of time past the stated expiration date, suggesting that the ETriN ions originate predominantly from ETN sample impurities.
Differentiation of Homemade ETN by IMS-MS
An ESI-MS spectrum of the in-house synthesized ETN, obtained by applying an appropriate IMS gating scheme to remove major ETN peaks (C4H7N4O13 – and [ETN + NO3]–), is shown in Supplementary Data, Figure S2. In this mode, only minor anionic species, originating most probably from sample impurities, are detected. These impurities include the previously putatively identified sulfate adduct of ETriN at m/z 336, as well as other unidentified species. These impurities can act as fingerprint signatures, and potentially be used to readily differentiate between various samples. Elemental composition could likewise be determined using accurate mass measurements and tandem MS. Specialized threat compound databases from such data could complement other forensically relevant information that is available.
High resolution/accurate mass MS combined with IMS is a valuable tool for analysis of HMEs. IMS-MS allows identification of the ion species generated during sample introduction that may be otherwise impossible if limited to IMS alone. We have found that IMS-MS spectra are similar to those collected on a stand-alone ETD system for characterization of HME samples. ETN ionized by ESI, CD, and 63Ni forms similar anionic species, analogous to PETN ions documented in the literature. Although ETN synthesized by relatively crude methods yields very similar IMS-MS signatures to purchased ETN standards, gated IMS and high-resolution MS have been used to identify minor ETN impurities that may be indicative of the chemical source and the synthetic methods used to manufacture the threat. This information allows successful differentiation between, e.g., commercial explosives from homemade formulations, which is of great utility for forensic and attribution purposes. We envision that comprehensive IMS-MS analysis of both threats and common background chemicals could also be used to improve threat identification and reduce false positive results that are often encountered in stand-alone IMS ETD systems.
This work was funded by JHU/APL Internal Research and Development. While approved for unlimited public release, it represents solely the position of the authors. Use or mention of a specific product or trademark does not constitute an endorsement. The authors thank Mark Osgood (Excellims) for assistance with the IMS-MS setup and Trang Vu (JHU/APL) for providing additional in-house synthesized ETN samples.
Supplementary material
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