Chromatography Forum

There is a grave problem of truthfulnes here. What do you do if a independent lab finds out that the analysis is faulty and then someone leaks the fact that you knew about it?
On the other hand, I see no problem for anybody to acknowledge that a better analysis gave different results which are irrelevant to intendet use.

I can add an example here from the good ol' days (1990s).

I was testing a sample of acetonitrile from a bulk shipment. It had a very high purity requirement. When using capillary columns of many varieties the purity was 99.95+%, not measuring the water content.

But when using a packed column, I found an impurity of 0.33% which was not seen on any other GC chromatography analysis.

Since several lots of acetonitrile showed this impurity and all at about 0.3% no concerns were raised. We were using the acetonitrile in the lab at that time, but later we began to sell it as a product intended for HPLC use.

Now the competition was claiming 99.9% purity but was selling the product which was 99.7% pure, as we were also.

We claimed the product was 99.9% pure by capillary GC analysis (which was true) and the customers were all happy, no complaints, the new lots were just like the old lots.

What should we have done?

In another product we had a purity of 60% but when we purified it to 95%, it did not work the same for customers. We had many complaints.

What should we have done then?

You tell me.

Rodney George
consultant

Whilst I like Peter's suggestion, reality will bite when somebody uses more resolution. I don't believe there's a simple solution.

If the clients are purchasing to their own, or a standard, specification, and your product still complies, you don't have a problem. If it doesn't, you wouldn't claim that it does.

If clients are purchasing product based on your specification, then you have a problem, but you can easily create a new specification for new clients to minimise future problems.

I would prefer to rewrite the specification, but if you are operating in a really competitive market, retraining clients to accept a lower % purity for the same product could be very difficult - especially if client's purchasing is performed by a administrative clerk.

It's a change that should be performed in consultation with your marketing department, but it should happen - because it's critical for mutual trust.

The issue of increasing sensitivity or different methods finding more impurities has been around since chemical analysis started. The conventional solution is to ensure that the specification establishes limits only for critical parameters, and to constrain the reporting of individual impurities to a nominal lower concentration ( eg 0.05% ), and fully defining the methods.

If assay is critical in a specification, it can be performed separately, usually against a reference compound or property. Assay is especially important with organics that may contain salts and other compounds that aren't detected by the analytical instruments routinely used.

I've also encountered the "increased purity - decreased performance" several times - often due to residual water or pH, but once when an amine precusor impurity was catalysing a desirable reaction.

Typically, we suggested to clients that they revert back to the cheaper grade, and our marketing people made sure that the crude grade was cheaper for that client.

For the amine, we didn't detail the impurity's identity on the specification, but defined the "Impurity A" content as "report". The client was happy, even though we said the impurity A content could change in the future, and wasn't controlled.

Well, I'm not getting updates on this topic for some reason, but it seems to have taken an odd turn. While the results he reports are not my problem (anymore, that is), it is the fact that I am the supposed 'heir-apparent' to his position (running the instruments that is, not the company!), and I'm really just chomping at the bit to change things around. Plus, he can be a bear to be around if you rub him the wrong way. For example, when I first started in the section, I started doing things with the instruments without asking him (as he was running my samples) and it must have irked him, because he didn't talk to me for a few weeks!

I really don't see this as an odd turn, the point is that there may be history behind the way things are currently done, and before wanting to change things it is worth finding out the way things are done the way they are. There may have been very good reasons why this way of doing things was chosen, and these reasons may or not be valid. As a newcomer to the company when you want to immediately change things without finding out the reasons things are done you can develop a reputation of not being a team player.

An employee of any company should be concerned with business aspects of a change in analytical methodology as well as the technical aspects. I have a very good idea of which of the posters replying to your post have a background in a small business and which ones have working in a academic environment or in a large company at a position far removed from profit and loss considerations. There is a very different way of looking at things when you are held responsible for decisions that directly affect the companies bottom line.

To me the first post indicated two different perspectives as to the reason the analyses are being performed, and a lack of communication and understanding of the other person's point of view on both sides.

I'm not really a newcomer, this has been going on for a couple of years. And belive me, I'm not the only one with an issue regarding the situation. It is a communication problem, and mostly because there isn't any communication. So for now, I bide my time, and bite my tongue.

bisnettrj2, I went back and read your original question: "My question: How do I go about showing him that the way he is running his instruments is a.) insane; b.) inefficient;, and c.) exceptionally annoying?"

Are his assays working and giving consistent and reliable results? Is he following the proper method? If so, then his methods are not insane, nor inefficient. As for annoying, tough luck there. We all do things which drive others crazy.

The way I would go about doing this is to gradually educate your co-worker the benefits to new/different techniques. We all are stubborn and when just told to do something different, we will keep doing the same. Wait for problems to come up (failed sample sets, poor chromatography, etc.) and use those moments to make suggestions (i.e. peak shape might be better with samples in 10% ACN instead of 100% ACN). Let your work speak for itself, and when others work doesn't perform to your level of work, managers will start to think what you're doing differently and implement it. Do what you need to do to get consistent and reliable results, and if that means stressing why you use equipment a certain way, then include that in the discussion.

Yea, well, he's not just a coworker, he runs the place, so he kind of gets to do what he wants - whether others think it's right, wrong, inefficient, or brilliant. Others' opinions are relatively irrelevant to him if they don't jive with his world view. And he doesn't take suggestions/criticisms well, so if he asks, I'll give him my opinion. Until then, I'll keep my gripes to myself.

I will disagree with you on whether his assays working mean he isn't being inefficient. And perhaps insane wasn't the correct term - perhaps illogical would have been more appropriate. I feel, and I think this goes back to Ron's point, that if he were more efficient, we could handle more business, and therefore make more money. And if we do that (which I've done in my analysis in the last couple years), then the powers that be might see fit (this applies to me, not him, obviously, since he runs the joint) to give a bump in pay. But, increased throughput for him means more to the company's bottom line, which is in his best interest too.

Like I said before, it's not the quality of the results - it's the way that he goes about getting them that drives me batty, along with the personality quirks. If I get the chance to proffer a suggestion, I will. But until then, I will keep it to me.

You wrote:

"And he doesn't take suggestions/criticisms well, so if he asks, I'll give him my opinion. Until then, I'll keep my gripes to myself. "

You answered your own question. Since he owns the place and it is his business, it is your business as an employee to follow all and every legal instruction he gives you. unless you want to find a new job.

best wishes,

Rodney George
consultant

Indeed. But the carrot has been dangled that I'll get to take over the instrumentation in the somewhat near future, so I need to be quiet until then. Then I can meddle with the analysis all I want, and in a few years someone will hopefully challenge my reasoning, and just maybe I'll remember this discussion and be open-minded about new suggestions.

If the same person is still a co-owner of the company don't count on being able to change anything you want when you have "control" of the instruments. It is a common misconception that when you are promoted you have more power to do things your own way, in many cases the meaning is you have more responsibility for the results but no more power to change things. If the person is such a control freak about the way things are done do you have any reasone to believe a new title will change things? I'm not trying to be discouraging, but you need to honestly evalute the situation and see if things do have the potential for real change, and if not evaluate your options.

I was once told by my supervisor the way I wanted to do things was wrong, nobody else believe in doing things the way I did, and if I didn't believe him I should check around the industry and see if anyone else thought I was right. Three larger, more stable companies agreed with me, I picked one, and now am living in a nicer house in a very nice part of the country and making more than double what I did with better benefits.

I have hope, Ron - and my mortgage balance/home value being what they are, I'm not moving anytime soon. So I'm making the best of it. But I agree, my odds of being able to change things completely are slim, but if he goes completely hands off, then I can do small things that won't be immediately noticeable. Incremental changes, if they go unnoticed, can amount to real change in no time. I hope!

In many cases incremental changes are best, change one thing and see if the effect is positive, negative, or no change. That way you have more of a knowledge base when the next problem comes along. It may seem to take longer, but small incremental changes can actually lead to a robust method quicker than changing a lot of things at once.

Good luck.

This is an important thread going on as there are essential issues of both product quality and analytical accuracy. A pervasive mind-set has been to "leave well enough alone"; yet some managers, (myself included) are tasked in our job descriptions with "developing analytical procedures that maintain company competitiveness, consistent with new and novel industry standards, and leading edge technology". Yet, these ''cutting edge'' methods may lead to a product being ''out of spec". Our approach has been to either alter the specs based on the new findings. We were audited in 2009 by FDA and inpsector asked me "how do you deal with discrepancies between expected vs observed specs?". I told her that "we investigate it, and at times alter the specs".