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HPLC for home use

Discussions about HPLC, CE, TLC, SFC, and other "liquid phase" separation techniques.

34 posts Page 1 of 3
I'm an out-of-work wet bench chemist who has never had the opportunity to run HPLC. I've taken HPLC continuing ed courses, but I need "hands-on" experience in order to get a chemistry job. For this reason, I'm thinking of purchasing a used system to work with in my home. Questions that come to mind are:
Which system and software to buy, for at home use?
Will I be able to purchase chemicals and solvents, as an individual?
What environmental considerations and/or legal regulations are there governing the home lab?
As a respected Dan Ramlose sent the following message I think there has been a change in your translation website or perhaps your computer has a virus or malware on it as your last several posts are not up to your quality (since sometime on May 10th).The posts in the following topics are meaningless:
HPLC for home use"
, a little redacted text.
We split it into paragraphs, Council made forward, history will move back, but the policy will give the smallest font.

1) Council
Purely IMHO - not money on chromatograph, spend money on job search and training courses.

There is an old bureaucratic adage "you're a small bug without notes [ sertificates , documents , recomendations] , but with notes => you is people". :twisted:


With him, all speakers agreed.

2) "Skazka loj, da v nej namek , dobru molodcu - urok. Ne lubo- ne slushaj , a skazivat ne mesaj" (c)
[Tale lie, so it hint, dashing boy - good lesson. You do not like- do not listen, don't stop tell.]

[b]His status but it was different[/b]. But you have this experience does not fit! :evil:

Of my friends did so only Professor Anatoly Petrovich Rodionov, God rest his soul *. :( :( :roll: He worked at the time at the Institute of Pharmacology in Moscow over a government grant and not was unemployed. **
Therefore, Rodionov had to divorce in the village home vivarium *** equipped with a guillotine, and extract metabolites whithout rats blood and analyze them in the home laboratory. But official results of all passed through the institute and the grant money as a result have been obtained through accounts of the institute.
Of the equipment he used UPLC "MiLiChrome" and hybrid from Czech Chrom and Pue-Unicam

Respectively, with the reagents had no problems - narcomanii (drug addiction as social problem) was not in the USSR in principle, even in the 199* milition ( police) looked at the chemicals freely. But now police lyutuyut****

And with spent reagent were not disposal problems - and spent reagents and dead rats burned and cremated in a Russian stove (oven) , so that waste is utilised of in the heat. :D

* So we talk about long-dead man-righteous
** Another question that the situation with operating in Russia under Yeltsin was like now to Côte d'Ivoire with Uatarroy.
"The work is easy to find, but just impossible to get the earned money" (quote from my friend colonel, who served in Abidjan in the peacekeeping mission).
It was discontinued funding of scientific work and money became scroll through the financial pyramid (MMM Mavrodi our analogue of your Bernard L. Madoff). In the country because of the financial pyramid was hyperinflation - the type of Weimar Republic, though not the same as in Zimbabwe. Salary gave out after many months, when the money is worthless.
Against this background, many researchers have gone into the business - sometimes very peculiar.
Thus the transfer of Professor Rodionov working on the house was not due to his love of science and not a "love rat torture" and the exceptionally difficult situation in the country. In order to obtain what the money had to work in unsuitable conditions
*** krysyatnik ( Rats-coop / rats-farme) - it joke but in any joke is a small part of joke.
As premises for the content of the rats used an old chicken coop.
You've got to make a clarification - the majority of Muscovites from the Soviet era a number of homes - an apartment in the city where they live permanently and dacha (village, country house) outside Moscow, to go for a weekend fry Shashlik ( barbecue) for example.

**** meaning
If you've seen both in the nature of the wolf pack attacks the sheep, scatters them and cut - a situation that you represent. Unable to cope with the traffic of heroin from Afghanistan, police "found the goats for the remission of sins" in the face of legally employed chemists. The problem with the fact that conventional chemicals are monitored by the police as precursors of drugs by the police - the total world. Google translate
I'd recommend against it. Even used, the equipment is not inexpensive, and you need the appropriate "infrastructure" to go with it: volumetric glassware, balance, pH meter, appropriate ventilation, etc.

Permits, etc. will depend on where you live. If you're in a rural area, you may simply "fly below the radar". In an urban area that's more difficult! Unless you stick with something like ion-exchange, you're talking about gallon jugs of toxic and/or flammable solvents.
Most chemical suppliers will not sell to individuals, so you will usually need a business license of some sort (and be prepared to answer questions from the DEA if you're in the US!).

I'd check with the major hardware vendors and see what they offer in the way of hands-on courses. I suspect that it would cost you a lot less in both money and effort. I'd also check with local community college or university labs. You might be able to volunteer as an unpaid lab assistant. If there is a chromatography discussion group in your area, join that and network like crazy.
-- Tom Jupille
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
Can't agree more with Tom.

The second hand HPLC system itself can be a hefty expense and there's no 100% guarantee it will work straight out of box. I had one second hand HPLC dead on arrival and it was incredibly frustrating to do the troubleshooting and pay for the parts that really needs to be replaced (arrrh you evil second hand equipment vendor/previous users). I know that may be one single case amongst many second hand equipments sold, however that experience was horrible enough to let me stay away from buying second hand systems for a while.

For chromatography software (CDS), popular ones do not come cheap. So if you want to get trained in using the software (for better employability) better register software training course from major vendors.

Apart from glassware and chemicals, you will also need a healthy stock of consumables and spare parts to make your HPLC experience (i.e. PM kits) happy and smooth. Unfortunately some of those did not come cheap either and vendors are likely to be reluctant to sell to individuals.

If you are on the *VERY CASUAL* side, Vodka and distilled water will give you a sense of strong/weak solvent and you may even use them to affect some separations :twisted: . However if you are planning to do some serious work I strongly advice against that practice!

As Tom said, if you are desperate for some hands-on experience consider a volunteer job in companies or university labs. Chromatographers are nice, nice people :D
The sources to which you and Tom steer me have not worked out. I've tried every one of them and have been turned down everywhere. I am understanding everything that I read about HPLC (the phases, the polarities, the delay volumes, dead volume, turbulence, band broadening, etc.) I have an MS in physical chemistry and 20+years researching wet chemistry methods. I need access to a machine. I can buy an older model reburbished major market instrument with upgraded major market software for $10,000. I've already spent 3 times that much in courses and programs to obtain HPLC training - and I still cannot get a chemistry job because all the employers demand "hands-on" (not just "ACADEMIC") experience.
Go to your local College/University and volunteer as a lab assistant...you will have use of all of their equipment and get your "hands-on" experience and an additional item on your resume... :lol: :) :D
If you are good with your hands and understanding of instruments, you can try another approach. Often instrument companies are looking for people to do field service work. And the field service guys are often tasked with giving inital training to new customers. A good showing in that kind of work can allow you to step over to applications support - or over into a job at a client company. And, having a job gives you an advantage in the job market.
I also think it is a bad idea for the reasons mentioned.

Furthermore, during interview you will be asked to provide more information on the context of your previous hands on experience. Saying that you bought equipment and self-learned will sound really weird and people might think that you did irrelevant things. Trying to say that you have previous experience without a relevant CV might also back-fire.

I have tried in the past to help individuals like you (because chromatographers are nice people :wink: ). In both cases, human resources had to have a talk with me. At one job, they said that it was a waste of resources and time, at the other work place, I was told about the dangers of accepting volunteers (other than students, or people affiliated with another institution -i.e. they already have a job-) due to labor laws (i.e. exploitation of someone that needs a job).

I know, chicken and egg situation!
I dunno. If I was looking to hire someone and they said they purchased, repaired, and put into operation a surplus analytical instrument in order to learn about a technique, I'd be impressed. And if you could actually verify an instruments operation, you could turn around and sell it for a profit. I've done this many times over the years and have in my personal inventory several instruments (including an HPLC). Many times, I've purchased instruments only to completely disassemble them and see how they were constructed.

Am I weird and doing irrelevant things, or do I actually love analytical chemistry so much I've made it a hobby? You decide.

The problem I see is one of risk of poor return on your money if you fail. Furthermore, as people have mentioned, there's the need for additional resources to make mobile phases and safety issues with handling solvents. You'd have a very hard time obtaining reagents without a business license.

It's an ambitious thought, but a better use of your time and money would be to get some get references on the technique and study them, and take a short course at an ACS meeting for example. There's no risk in that.

- ender
Maybe "weird" was a poor choice of words, probably "atypical" would be most appropriate. In terms of relevancy, someone that has worked for a year or so in a lab, using HPLC instrumentation, they have probably used an array of different columns to separate/analyze compounds of interest and start having a feeling of HPLC method development. How far would you be able to go at home with let's say an LC-UV? Maybe construct a calibration curve by using caffeine, and measure caffeine in different liquids?

I would for sure give an A for effort...

Maybe this is the right place to instead require for a volunteer position in someone's lab? If you have enough money to buy an LC-UV to play around, probably you have enough to temporarily relocate if necessary and spend some time to someone's lab. I think we all agree that motivation is not something you are lucking...
Kostas: I have a sister living in Phoenix with whom I could stay indefinitely for an "apprenticeship" in order to learn HPLC, but you have already indicated that HR will not allow you to bring an eager pupil like me into the lab. I want to re-iterate to those who keep suggesting more courses, that I have taken two ACS-sponsored HPLC courses, two Agilent courses, (one on equipment maintenance and the other on ChemStation including "3D"), that I have read all or part of 4 major HPLC books that I purchased (including Snyder & Kirkland), that I also attended 2 ACS-sponsored courses on mass spec in which I glimpsed the possibilities unleashed by deconvolution and data-base mining, and that the Instrumental Analysis professors at two major universities have turned me away saying that I'm ready to "operate" an HPLC. To those who say that I could learn little at home, I would answer that I could learn the software and equipment assemblage, while operating principally in isocratic mode, recycling salvaged solvent with the appropriate device. I could experiment with various pre-filters, attempting to pre-purify whatever I load. And finally, I could experiment with gradients (the solvent guzzling technique) on some mixture of peptides, fatty acids, petroleum products or a standard mixture that I might purchase. It appears that I can buy ACS-grade methanol; if that is the case, I can purify it, degas it with my membrane degasser, and run gradients with it and purified water.
Boolie, I have accepted 6 internships for this summer (one high school and 5 undergraduates) beginning June and I am at capacity in terms of mentors and office space. We could though shoot for August and afterwards. I do not make any promises but if you send me an e-mail, clearly indicating that you want to volunteer for an internship where I work and how that will help your career, I'll see what I can do. Refrain from mentioning in the e-mail that you are looking for a job. Just focus on what you can learn and how invaluable that would be.

Again, I do not want to get your hopes up, and I do not have an opening but I can maybe help you through an internship to acquire some hands-on experience. I am sure that we will have a couple of projects that will need to be brought to completion from our previous interns.
You originally asked:
1. Which system and software to buy, for at home use?
2. Will I be able to purchase chemicals and solvents, as an individual?
3. What environmental considerations and/or legal regulations are there governing the home lab?

1. Which system and software to buy, for at home use?

If you can't find anyone local to work with (where are you located, btw?), and you're stuck on buying an LC, I would definitely go for either an Agilent 1100 or a Waters Alliance. If Agilent - I would look for an MWD or a VWD, unless you can get a good deal on a DAD, but then make sure the Chemstation software has the Spectral tools module included. If Waters, then make sure the system comes with Empower (note: I don't and haven't used any Waters systems, so I'm not sure if you would need any special add-ons to Empower if you get a PDA).

2. Will I be able to purchase chemicals and solvents, as an individual?

You've stated you can find ACS methanol. We all know you can get ethanol:water mixtures and distilled water at the local supermarket. If you can get your hands on acetonitrile, then you would be in business, solvent and system wise.

You can probably obtain HPLC columns from eBay (buyer beware). There are a few people on eBay that seem to regularly sell HPLC columns, usually starting around $75 each. Replacement parts can probably be obtained through the manufacturer or, again, through eBay.

Obtaining analytical standards is probably going to be hard, outside of what are available to consumers (caffeine, ibuprofen, various herbicides like glyphosate, etc.).

3. What environmental considerations and/or legal regulations are there governing the home lab?

That will be up to your local and state regulators.


How exactly you're going to do to get your hands-on experience, is another thing altogether. I would probably try to follow a USP method for purity of household medicines (ibuprofen, maybe?). Or possibly an EPA drinking water method with UV detection (EPA 532, maybe?). You will need to possibly invest in the various extraction systems in order to show that you can completely follow a method, and you should be able to show that your results meet the QC criteria set out by the various regulatory bodies that govern the implementation of the method. However, you will be working outside a regulatory agency's certification or licensing, so your results may mean nothing to a regulated lab.

Will this help you get a job? Maybe, maybe not. It may show that you are proactive and can work independently and may show you have the necessary skills for the job. However, it may be interpreted as highly desperate, and might be indicative of poor decision making (this will be a *lot* of money to spend to get a job). As Kostas and Tom and others posted, this is definitely not the "normal" way to go. But it might work, and who are we to tell you you're wrong?

If you can wait for Kostas' offer, I would take it, if he's able to offer you a spot. Or, maybe you can re-enroll at the local university in an analytical instrumentation class that has an HPLC unit - at least you would get some hands-on experience there, if not a lot. Maybe you can talk the professor into letting you do extra lab work, or as a student you can find a professor doing research, and volunteer to help him in exchange for the experience. As a student, the university should look on you with more acceptance than as an outside individual.
Time flies like an arrow. Fruit flies like a banana.
Having been on the reading resumes end: Experience someone gets at home is interesting - but unless it is part of a successful business or has resulted in publications in peer reviewed journals, it does not show ability to do anything useful. I have no reference to call or transcript to review to see how you did and I am not going to take the time to review work done at home to see if you did it correctly or understand what you did. I have worked with people who have been self-taught (on the job) - and the fact that an employer sees valuable results from that self-teaching indicated that the person got it right enough for someone to pay for it. The point is that I need a reference point to evaluate that previous learning, whether from a previous job or from a school.

Second point on the resumes reading end: These days there are some very good chemists out of work. I really prefer to read the resume of someone who is leaving an organization voluntarily. Second choice is someone who has been separated from previous employment recently. The shorter the time since last employment, the better. The longer the time since last employment – without some other information (like personal knowledge of the situation or recommendation from someone I trust) the indication is that this is someone that nobody else wanted to hire. Thus – as quickly as possible get to a paying job of some kind or into a situation where someone can recommend you to an employer through their network. It is truly easer to get a job when you have a job. (I've done it both ways.)

Third point from the reading resumes end: I read the cover letter to see if you match the position. I read the resume to see why I should NOT hire you. I look at the chronology to see where you have been and what kind of track record you have (and will put dates in order if the writer has used a non-chronological format). I look for missing experience, job history, and credentials. And, I read between the lines to see what you are not telling me. For example: If you have worked for a company for 20 years and take some time off to have some fun before going on to the next job. The fact that you have 20 years with one company is a big plus – it tells me that you have maintained the trust of your previous employer that long. If you take make a large capital investment (like purchasing an instrument) and take a couple of years to learn it – I have the question: Is this a failed business venture – and the guy is not being straight with me? Part of my job is to protect my company from risk – including hiring someone who hedges his answers -- as well as the mad scientist who does dangerous stuff in his basement. (If you purchase an instrument and tell me that you have learned it in six months, I'm going to have a hard time believing you right up front. This stuff takes time, even with guidance.) And, if the resume shows a change of positions every two years, I will be looking for anything that indicates whether this whole story is an issue of poor judgment or poor luck. (And I have noticed that people with poor judgment are sure that it is poor luck, so I have to figure it out.)

Understand the hiring process to evaluate the path you are looking at against other possibilities. Be sure that what you want to add to your resume is really a plus and you can do it in a way that does not raise red flags. Not everybody reads a resume the way I do - but this is what I have learned to do from others, so I assume the method of questioning is not uncommon.
Boolie, I have accepted 6 internships for this summer (one high school and 5 undergraduates) beginning June and I am at capacity in terms of mentors and office space. We could though shoot for August and afterwards. I do not make any promises but if you send me an e-mail, clearly indicating that you want to volunteer for an internship where I work and how that will help your career, I'll see what I can do. Refrain from mentioning in the e-mail that you are looking for a job. Just focus on what you can learn and how invaluable that would be.

Again, I do not want to get your hopes up, and I do not have an opening but I can maybe help you through an internship to acquire some hands-on experience. I am sure that we will have a couple of projects that will need to be brought to completion from our previous interns.
__________________________________________________________________________
Thank you Kostas - I am interested in pursuing your offer of an "internship". I will be touch within the next few days, I guess the best route is via your "linked-in" address? ---Boolie [jharrington24@my.stlcc.edu]
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