benzylchloride1 - 5-12-2007 at 20:10
I am building a simple HPLC system. I have purchased a Beckman model 332 controller, Beckman model 110A solvent metering pump and a Beckman model 153
analytical UV detector. Where I could I obtain manuals for the installation and use of this equipment? I know that I am going to have to buy more
equipment to get this instrument system running. I am a high school student that is currently enrolled at the local university and majoring in
chemistry. I am currently taking organic chemistry; my favorite class of all time. I have a chemistry lab at home and i am also working on a simple
gas chromatography system for my home lab.
Sauron - 5-12-2007 at 20:38
You might try Beckman itself for starters.
Failing that try advertising (for free) on LabX,com
One free ad per item so you may need to run 3+ ads. If you run a single add for three different manuals they will want money.
Congratulations on the chutzpah to take this step.
When faced with same step I found a big name HPLS equipment maker whose documentation was available for download, so I could study it before buying
anything, and who has local representation in case I need help or spare parts or service.
For those reasons I went with Waters and now have half a dozen analytical and preparative systems and machine control via IEEE bus and Millenium32
software on Windows PC.
Not being familiar with Beckman HPLC models, are yours isocratic or multisolvent? What is max pressure the system can handle (should be c.6000 psi)
I also waited till the dust settled before starting to acquire columns.
At the minimum you will need HPLG tubing (usually stainless steel) and fittings and tools. It is quite likely that your UV detector will need a new
lamp, it is very likely to be a D2 lamp and a new one will set you back at least $400. Expect to have to replace it every 6-12 months. Hopefully I do
not have to tell you to never touch the bulb with your bare hands and NEVER look at it when it is operating. If your detector is well designed, this
will be impossible. It could blind you.
You will find service and repair expensive if available at all.
You will find spare parts expensive if available at all.
I have equipment that in some cases Waters no longer supports and I just buy extra working units to cannibalize as needed because it is cheaper to do
that than to buy new spares!!
Another caution: HPLS systems operate with organic solvents at high pressure. A bad tubing connection can not only drip but spray a high pressure jet
of the solvent. ALWAYS assume that such a leak will happen and ALWAYS assume it will head straight for your face. Wear face shield, and a Tygon lab
coat. SOme HPLC solvents are less than user friendly. Do not wear them!
Good luck with your adventures in HPLC. It is a powerful seperative tool.
Sauron - 7-12-2007 at 02:09
CORRECTION
The Beckman 153 UV detector does not use a D2 lamp, but an Hg lamp.
An inferior UV source but a lot cheaper. $183, as opposed to c.$500.
http://www.mcphersoninc.com/lightsources/lightsourcelamps.ht...
benzylchloride1 - 10-12-2007 at 09:11
Thanks, I was able to get a hold of Beckman and they are willing to find the manuals for me. I was able to get this system of of ebay for under$150.
All the equipment turns on and was said to be in working condition. I bought a face sheild ,so I plan to wear it when working with my new HPLC system.
I have a solvent distillation head and I plan to use this to purify the solvents. What solvents are good to start with for general use?
Sauron - 11-12-2007 at 00:25
Until you get used to working with the ferrules and tubing and get your plumbing perfect (no leaks) the only fluid that you should be using is HPLC
grade water. Once you are ready, you will need HPLC grade solvents. You basically cannot purify and reuse HPLC solvents. Maybe with a spinning band
still, but nothing less. HPLC solvents are expensive. But anything less will ruin your work and/or your system.
Expect to need to replace plungers, seals, etc. not to mention that Hg detector lamp. Spare parts are expensive. HPLC can be a money pit. I probably
have $50K US in mine.
The choice of solvent(s) depends entirely on the nature of your anylate. Is the system isocratic (single solvent) or capable of binary, ternary or
quaternary mixtures (gradients)?
Methanol, acetonitrile, nitromethane, there are dozens of commonly used HPLC solvents and one size does not fit all. Look at the diversity of column
packings as well. The two must be considered together. Even for simple isocratic systems, when one is polar the other will be nonpolar. And vice
versa. This is what normal vs reversed phase is all about.
Also get yourself DryLab software, HPLC simulator, it will teach you a lot.
not_important - 11-12-2007 at 08:22
Just a FYI - this is an example of what is used to recover/purify solvents for HPLC
http://www.solvent--recycling.com/hplc_solvent_recycling.htm...
this is a bit fancier than your typical home lab distillation rig.
I'll second Sauron on the simulator software, either that or a resident HPLC technician.
Sauron - 11-12-2007 at 08:27
If your pump is isocratic (as I suspect) then there is a simple trick to economize on solvent. A solvent recycling system lets you return solvent in
between peak to the solvent reservoir. For a lot of seperations this can be a very significant percentage of the total solvent used.
Obvious you need to stay well away from peak tails.
And yes B/R are the top of the heap, king of the hill in spinning band distillation systems. For labs that do a lot of HPLC one of those automated,
PC-controlled stills can pay for itself in short order despite a price tag in the $25K-$50K range. HPLC solvents are not cheap. A single prep scale
seperation on a few grams scale can use 10-25 liters of HPLC solvents. Do the math.
[Edited on 11-12-2007 by Sauron]
benzylchloride1 - 12-12-2007 at 10:51
I just received the detector, the lamp is in working condition. The system is an isocratic system. The pump turns on and responds to the controls. I
cannot get it to pump distilled water through the system. I am currently looking for the Dry Lab HPLC simulator software. Is it free ware or do you
have to buy it?
Drunkguy - 6-2-2008 at 14:17
Ah, here is the thread Sauron directed me to.
I hope the real chemists can continue to push the boundaries of their laboratories.
After my recent aquisition of a Flashmaster II puification system, I am greatful to finally be at the interface of computer meets machine.
Sometimes in the race to make compounds for the first time, its possible to overlook the fact that mixing the chemicals together is really still at
the left of the chemical arrow that consititutes an equation.
In order to get products, an important and necessary step is to analyze the composition of the crude product, before making an informed decision about
how to proceed.
biochemist - 6-2-2008 at 19:59
RP-HPLC experiments were the last thing on my mind during high school! What are you planning on doing with this anyways?
benzylchloride1 - 21-2-2008 at 17:21
I plan on using this HPLC system to analyze reaction product from experiments I conduct. I was able to obtain the manuals for free from Beckman. The
system is currently almost operational. I just need to buy some columns, filters and 200 mm chart paper for the recorder. The paper is obtainable from
Cole- Parmer, but is ridiculously expensive.
benzylchloride1 - 22-2-2008 at 20:40
I was able to buy a new Waters Symmetry reverse phase octadecyl column off of Ebay for $25.00. I was able to prime the pump on the HPLC system and the
pump fully responds to the controls. The system is working, almost.
Ephoton - 25-2-2008 at 14:41
sauron has way to much bloody money ;P