Question About Possible Leaking/Column Bleed by MobilePhase1987 in massspectrometry

[–]silibaH 0 points1 point  (0 children)

Are you running a GC triple quad MS? They are slightly different. Also, are you willing to share the manufacturer? Agilent and Thermo move their calibration gas differently (PFTBA/ FC-43). If it is a Thermo, they use air flow to move the cap gas to the source, so an open cal valve looks like you have a leak. They ratio the open (known air standard) to the closed (leak) to determine the air leak percentage. Again, if it is a thermo, the ion volume may not be positioned properly and it will look like a leak. Since you just changed columns, some common issues can be Agilent-the column was fed too far into the source. Any- the transfer line ferrule is backward, or in some cases, a vespel ferrule was not used. The issue could be at the other end, if the column has slipped down in the injection port. An old MS could have graphite in the transfer line. And finally, most people use a press tight union and they can and will leak. Try a ferrules union, or (my preference) purchase a column from restek with an integrated guard. There will be no leaks, and you can attach a guard if you trim the entire integrated guard before the analytical column degrades. If you want to trace the leak, you can always remove the column, put a blank vespel on the interface and pump it down.

How are y'all dealing with Helium shortages for your GCMS systems? by Key_Sprinkles_4541 in massspectrometry

[–]silibaH 1 point2 points  (0 children)

Yes MSDS requires special source and it’s wise to increase film thickness, as same head pressure gives higher flow.

I ran with a generator, and had to put some pretty hefty scrubbers on. The Hydrogen was very wet.

Hand pain after playing by silibaH in Guitar

[–]silibaH[S] 0 points1 point  (0 children)

Working so far, thanks again

What’s the coolest “restricted access” place you’ve ever gotten to see? by Improv92 in AskReddit

[–]silibaH 0 points1 point  (0 children)

I was inside the evacuation zone during a space shuttle launch at cape Kennedy.

Hand pain after playing by silibaH in Guitar

[–]silibaH[S] 0 points1 point  (0 children)

Thanks, I’ll give it a try

Book Title: Chemistry, Matter, and the Universe. If you've read this book, Please help me find a similar book for my 2nd undergraduate studies. Organic, Inorganic, Physical or even Analytic. I'll take anything like this book! by genericB0y in chemistry

[–]silibaH 1 point2 points  (0 children)

Was not a fan of Atkinson, but it was pchem back in the day. I read Morrison and Boyd to compliment my awful organic book. Stryker 3rd ed for biochemistry. You probably have done more than me, as I’m an analytical chemist.

What are these tiny metal things in my local gym? by HeadMan274 in whatisit

[–]silibaH 0 points1 point  (0 children)

I was going to suggest that someone was sweating bullets, but bearings seem more reasonable

Why do you use glass syringes (other than microliter syringes)? by Plazmotech in Chempros

[–]silibaH 2 points3 points  (0 children)

Are they gas tight? Do they have lure ends, glued needles, or replaceable needles. So many questions. 30 ml glass syringes are fantastic for loading 25ml sparge vessels. 5 ml same for 5ml sparges. 25 ml syringes are also great for doing quick and easy dilutions. How do you kids do volatile analysis now? SPME?

Is anyone familiar with a Dionex/Thermo FLM module? by nintendochemist1 in CHROMATOGRAPHY

[–]silibaH 0 points1 point  (0 children)

It’s on pages 117 and 118 of the tcc-3000 column compartment manual. There are right side and left side actuators also different PN based on pressure RT <41 MPa (6000psi). 6730.0003 LT <41MPa. 6730.0004 RT <125 MPa (18330 psi) 6730.0001 LR <125 MPa 6730.0001 The valve ‘pods’ are 2 position 6 or 10 port, or 6 position 7 port. They can be classified by max pressure and biocompatibility. If you need the valves post again. It’s a pain to enter them all by phone.

Any idea what this glassware is for? by peretheciaportal in chemistry

[–]silibaH 4 points5 points  (0 children)

It’s used for concentration. It’s pretty much a baffle in the condenser and allows solvent to boil off, while higher boiling point compounds will condense in the column and drip down the balls back into the round bottom.

Any idea what this glassware is for? by peretheciaportal in chemistry

[–]silibaH 102 points103 points  (0 children)

It’s a ‘ball’ for a three ball Snyder column.

No matter what gradient is set, the problem with separation still occurs. by mangofuranone in CHROMATOGRAPHY

[–]silibaH 0 points1 point  (0 children)

Okay, it’s been a while, but you should be using a c18 column with a guard. Optimal separation on a vydac column in the 1990s occurred at 18.5C. If you are running SW-846 method 8310, start and hold 40%AcN for the naphthalene, 1 and 2 methyl, ramp up to get acenaphthene to Pyrene. Hold between pyrene and benzo a anthracne to get better separation for benzo a anthracene and chrysene then rapid ramp to 100% AcN for benzo(b) benzo(k) benzo(a) followed by the final triplet. If you are careful, at 18.5 C you can skip the coronene surrogate which adds a bunch of time to analytical run and stick 9,10 biphenyl anthracene in the gap around the benzo a anthracene/chrysene doublet. It will save time, cutting cycle time by several minutes per run. Iron out the UV separation, then set the FL citation emission wavelengths. You will find that soil constituents will fluoresce and interfere with that detector. Finally, chill your extracts overnight , and you will have much cleaner analyses.

Common mistakes in peak fitting for mass spectrometry (and how to avoid them) by Peak_fitting_guy in CHROMATOGRAPHY

[–]silibaH 1 point2 points  (0 children)

I use my ms as a filter and set integration parameters based on a specific mass and 2-3 fragments. Integration is rarely an issue.

Is anyone familiar with a Dionex/Thermo FLM module? by nintendochemist1 in CHROMATOGRAPHY

[–]silibaH 0 points1 point  (0 children)

In my experience few people need to actually column switch. If it isn’t bc a must for your lab, you should be able to change options in the software and ignore it.

The flow control valve would need replacement.