Ed Dabrea, Technical Director, with Jupiter's dual HP Micro-ECD GC system

Anatomy of a breakthrough "The detector was behaving mysteriously. If you look at the empirical data, it was not consistent. I wanted to find out what was going on." Mahmoud Abdel-Rahman, R&D engineer at HP's Little Falls Analytical Division in Wilmington, Delaware, is discussing what drove him to investigate the performance of the electron capture detector (ECD), a mainstay in food, pharmaceutical and environmental labs around the world. Mahmoud's investigations into the mysterious behavior of the ECD led to the first major redesign of the detector since its introduction 30 years ago. Recognizing that the inconsistent results were standing in the way of any improvements whatever, Mahmoud began by developing a system for mixing the sample with the detector gas before it goes into the detector. From that point forward, he began to obtain repeatable results from the standard detector. He then spent six months working out a mathematical model for the response of the detector, along with another model for its noise. "The common belief was, if we reduced the amount of the radioactive source, it would increase the minimum detectable level of the detector, that is, reduce its sensitivity." Mahmoud's model contradicted conventional wisdom: reducing the radioactive source would actually increase sensitivity. Reducing source size enabled the reduction of cell size as well, which in turn meant shorter run times. Recruiting a few volunteers working in their off hours, Mahmoud set up a classic "skunk works" project. Skunk works are an ancient and honorable tradition at HP, and his management encouraged him. "They wanted to know, could we improve it, or should we just forget it." He and his team built three different prototypes and demonstrated that his model worked in practice. He spent another year refining it before releasing it for production. "Reducing the amount of radioactivity enabled me to improve sensitivity and correct linearity," Mahmoud recalls. "But to improve detector stability, I had to look into the direct current (DC) model of the detector. This model told me that there are uncontrollable motions of electrons and ions within the cell that makes the baseline wander." The solution: remove the anode from the plasma and control the signal collection in the cell by pulsing the anode harder. The result is the HP 6890 Micro-ECD, the first major design innovation in ECDs since the inception of the detector. To get some idea of just how improved the instrument is, Mahmoud has provided the following comparison chart:

IT'S NO SECRET that hard times have fallen on the environmental laboratory business. Over the past year, some of the country's biggest labs have closed their doors. Others are retrenching. The sound you hear throughout most of the industry now is the chop of downsizing activity taking place as labs adjust to the new realities of the marketplace: tougher competition, lower rates, higher customer expectations and relaxed regulations leading to reduced analytical activity.

One lab defying the odds in a state where things have gone especially wrong for the industry is Jupiter Environmental Laboratories, of Jupiter, Florida. According to Jupiter's Technical Director, Ed Dabrea (pron. Da-bray), the political climate precludes an activist approach to environmental regulation. "Florida is wide open now," he says.

In spite of the market conditions, Jupiter opened its doors two years ago and has been prospering ever since. Interestingly, the lab was formed by Glynda Russell, a land developer who required fast turnaround on samples from property she was selling. As an entrepreneur, Ms. Russell was amazed to find an entire segment of the market run by people who seemed completely unaware of the needs of their clients and the nature of their deadlines. "They had the attitude that, well, your sample's in-house, we'll try to have it out by Friday," says Dabrea.

Glynda Russell founded Jupiter to meet customers needs in environmental testing

Russell recognized a niche opportunity and jumped on it. "She decided the way to exploit the situation was to have a lab that specialized in organic testing and utilized the latest technology to control overhead," Dabrea recalls. By dealing only with top-tier engineering clients and employing only senior chemists, Russell felt her lab could offer superior service and rapid turnaround at competitive prices.

Recruiting top chemists from other laboratories who were tired of working in poor conditions with old equipment, Jupiter Labs opened its doors in 1995, offering a three-day turnaround. They've never missed a deadline.

Six chemists, no waiting

The entire staff of Jupiter consists of six chemists. "We cut out bureaucracy," Dabrea explains."There's no hierarchy. Whoever answers the phone answers the phone. If the sample needs to be extracted, it is. We're very efficient at getting the samples through the lab quickly. We have short run times, so our capacity is very high. We use narrow-bore columns together with the latest mass spectrometers to eliminate sample reruns. The samples come in and instead of being stored they go right onto the instruments. We clear the instruments out every day to maintain total capacity as we go along. There are no hold-ups, no bottlenecks."

"We have clients who need same day rushes and we do that easily, too," Dabrea continues. "We will actually go out in the field and pick up the samples, bring them to the lab, and deliver the data by 5 o'clock."

Jupiter's quality service extends to difficult samples and unusual compounds that are not normally found in the EPA methods they customarily run. They perform many specialty analyses. They are completely automated and networked, monitoring and changing runs from home if necessary.

Each chemist performs whatever tasks are necessary to ensure their customers get on-time results

"We have a commitment to provide the very best service," says Dabrea. "And that's why we have all brand-new HP equipment." Their instrument component includes two HP 5973 mass spectrometers, one for volatiles, the other for semi-volatiles. But it's the new HP 6890 Micro-ECD, used at Jupiter for pesticides, herbicides, PCBs and multi-component compounds, that draws the raves (see sidebar, "Anatomy of a Breakthrough").

"The dual ECD is so incredibly sensitive, I've never seen anything like it before," says Dabrea. "Cliff Ross, our lab director, ran a one-ppb standard while I was looking at the actual counts on the side." Cliff says, "Look at these peaks, this is unbelievable, they're huge and sharp." The unprecedented results had me checking the standard logbook, looking for a dilution error. No mistake there. That day we changed the lab's low range for calibrations."

The HP 6890 Micro-ECD routinely detects compounds in the parts-per-trillion range, with a linear range greater than 5 x 104 for lindane.

HP Field Engineer Jeff Downing also loves this instrument, for obvious reasons. "It's a real easy sell," he says. "When you can tell people - 'I'll give you four orders of linearity, I'll give you sensitivity that nobody else has, and I'll give you stability of the detector to live through nasty samples' - that's a done deal. Now you're talking about where to go for lunch."

Dabrea says he can always tell if a client is knowledgeable or not. The ones who are will call him back as soon as they see the chromatograms from the micro-ECD. They're always incredulous. "They'll say, 'Don't tell me this is an ECD. It's impossible.' The baseline is absolutely flat, the peak shapes are symmetrical, the pesticide isomers are baseline separated. So it's a real joy to use. And it's very dependable," Dabrea goes on. "I get within 0.010 minute easy from run to run. So I can count on the same peak at the exact same time all the time, I don't have to worry about it fluctuating from day to day."

Jupiter has clients that are looking for extremely small concentrations, well below the federal regulations, in order to characterize their sites. Given the lab's approach to the business, the HP 6890 Micro-ECD provides the kind of performance the lab requires.

It is, in fact, the kind of enabling performance that any lab will have to acquire if it wants to compete in today's marketplace, given the new realities. Nothing less will do. Jupiter Environmental Laboratories can confirm that.
 
To obtain more information about the HP 6890 Micro-ECD, including on-line application notes, hardcopy literature, and automatic e-mail updates, click here.