EQUIPMENT August 2007 LaboratoryEquipment.com Featured New Product YOUR SOURCE FOR TECHNOLOGY NEWS, TRENDS AND APPLICATIONS Special Feature by Bernard Tulsi Trace Moisture Analyzer for Ultra-High Purity Gases Mini-Cavity Ring-Down Spectroscopy Analyzer Covers Wide Dynamic Range Read more on page 11 Biofuel Production Ups Demand for Analysis Instruments Part 2—Smarter Instrumentation Requires Better Training, Service and Support The emphasis in the United States is on bioethanol while in Europe it is biodiesel,” says Dave Armstrong, chemical and semiconductor mar- keting leader with PerkinElmer. “There tends to be more and dif- ferent tests on biodiesel than on bioethanol,” he adds. Bioethanol analysis makes extensive use of liquid and gas chromatography. Liquid chromatography is primarily used to measure the amount of unfermented sugars from feed- stock, such as corn or sugar cane, present in the fermentation vats at different time points during the transformation to ethanol. A significant amount of the fuel producers’ capital is tied up in the containers and in the process, which can go on for weeks, accord- ing to Armstrong. “So fuel manufac- turers want to gauge the rate of fermentation carefully to ensure the intended level of sugar has been converted to ethanol. “Once this happens, they distill the ethanol solution yielded during the fermentation process and then use gas chromatography to meas- ure the purity level of the ethanol,” says Armstrong. Gas chromatography is also used encompasses biofuels, often draw- ing on expertise acquired from a long, fruitful and ongoing associa- tion with the petroleum fuels industry. Oil refineries buy about $1 billion in laboratory instrumen- tation annually, including some 20% of all the gas chromatographs made in the world. “Bioethanol, based on the num- ber of gallons produced per year, is a bigger industry than biodiesel. “N ew construction of bioethanol and biodiesel plants is continuing at a vigorous pace with laboratory services needing to match this growth,” says Jim Mott, Ph.D., senior technical support specialist with Shimadzu Scientific Instruments. Dr. Mott adds, “The need to do basic instru- mental analysis at biofuel production laboratories will continue to press the need for more analytical equipment.” An impressive repertoire of ana- lytical instrumentation built on enabling techniques like gas and liquid chromatography, infrared (IR), and titration methodologies forms the nucleus of the test and measurement arsenal now de- ployed in the biofuels industry. Several analytical-tool developers and marketers now serve the “hy- drocarbon processing” sector, which T iger Optics LLC has introduced the HALO+ ™ , a mini-Cavity Ring-Down spec- troscopy analyzer capable of measuring at parts-per-trillion (PPT) levels. The new analyzer addresses the heretofore-unmet need for fast, accurate, calibration- free measurement of moisture in the parts-per-trillion (PPT) to parts-per-million (PPM) range. Companies in industries including semiconductor fabrication, labora- tory calibration and industrial Sponsored by www.ni.com Results are based on an E-mail survey conducted in May 2007. 0 – 20% of purchases are made through distributors 17.8% 22.2% 21.8% 12.3% 21 – 40% of purchases are made through distributors 61 – 80% of purchases are made through distributors 81 – 100% of purchases are made through distributors Survey Says… When asked what percentage of their laboratory purchases are made through distributors vs. vendors, our readers report: continued on page 12
Transcript
E Q U I P M E N T
August 2007LaboratoryEquipment.com
FFeeaattuurreedd NNeeww PPrroodduucctt
YOUR SOURCE FOR TECHNOLOGY NEWS, TRENDS AND APPLICATIONS
SSppeecciiaall FFeeaattuurree by Bernard Tulsi
Trace MoistureAnalyzer forUltra-HighPurity GasesMini-Cavity Ring-DownSpectroscopy Analyzer CoversWide Dynamic Range
� Read more on page 11
Biofuel Production Ups Demandfor Analysis InstrumentsPart 2—Smarter Instrumentation Requires Better Training, Service and Support
The emphasis in the United Statesis on bioethanol while in Europe itis biodiesel,” says Dave Armstrong,chemical and semiconductor mar-keting leader with PerkinElmer.
“There tends to be more and dif-ferent tests on biodiesel thanon bioethanol,” he adds.
Bioethanol analysis makesextensive use of liquid andgas chromatography. Liquid
chromatography is primarilyused to measure the amount of
unfermented sugars from feed-stock, such as corn or sugar cane,present in the fermentation vats atdifferent time points during thetransformation to ethanol.
A significant amount of the fuelproducers’ capital is tied up in thecontainers and in the process,which can go on for weeks, accord-ing to Armstrong. “So fuel manufac-turers want to gauge the rate of fermentation carefully to ensurethe intended level of sugar hasbeen converted to ethanol.
“Once this happens, they distillthe ethanol solution yielded duringthe fermentation process and thenuse gas chromatography to meas-ure the purity level of the ethanol,”says Armstrong.
Gas chromatography is also used
encompasses biofuels, often draw-ing on expertise acquired from along, fruitful and ongoing associa-tion with the petroleum fuels industry. Oil refineries buy about$1 billion in laboratory instrumen-tation annually, including some20% of all the gas chromatographsmade in the world.
“Bioethanol, based on the num-ber of gallons produced per year, isa bigger industry than biodiesel.
“New construction ofbioethanol and biodiesel
plants is continuing at a vigorouspace with laboratory servicesneeding to match this growth,”says Jim Mott, Ph.D., seniortechnical support specialistwith Shimadzu ScientificInstruments. Dr. Mott adds,“The need to do basic instru-mental analysis at biofuelproduction laboratories willcontinue to press the need formore analytical equipment.”
An impressive repertoire of ana-lytical instrumentation built on enabling techniques like gas andliquid chromatography, infrared(IR), and titration methodologiesforms the nucleus of the test andmeasurement arsenal now de-ployed in the biofuels industry.
Several analytical-tool developersand marketers now serve the “hy-drocarbon processing” sector, which
TigerOptics
LLC has introduced the HALO+™,a mini-Cavity Ring-Down spec-troscopy analyzer capable ofmeasuring at parts-per-trillion(PPT) levels. The new analyzeraddresses the heretofore-unmetneed for fast, accurate, calibration-free measurement of moisture inthe parts-per-trillion (PPT) toparts-per-million (PPM) range.Companies in industries includingsemiconductor fabrication, labora-tory calibration and industrial
Sponsored by
www.ni.com
Results are based on an E-mail survey conducted in May 2007.
0 – 20% of purchases are made through distributors 17.8%
22.2%
21.8%
12.3%
21 – 40% of purchases are made through distributors
61 – 80% of purchases are made through distributors
81 – 100% of purchases are made through distributors
Survey Says…When asked what percentage of theirlaboratory purchases are made throughdistributors vs. vendors, our readersreport:
continued from front coverby biodiesel manufacturers tomeasure the amount of glycerinin the fuel. Armstrong explains,“Biodiesel production starts withan oil. In the U.S. it is typicallysoy bean oil while in Europe it issunflower or some other seeds.
“As these oils become con-verted to biodiesel, glycerin isgenerated as a byproduct, which,if left in the biodiesel fuel, canraise the freezing point of thefuel and clog fuel filters.”
Diesel fuel tends to thicken incold weather. If glycerin is alsopresent, and this is more likelywith biodiesel, the problem canbe greatly exacerbated.
Biodiesel producers also testfor minerals such as sodium,potassium, calcium and magne-sium. When present, these minerals can form a soap-likesubstance and present problemssimilar to those with glycerin.“There is also concern over thepresence of phosphorous inbiodiesel,” adds Armstrong. “Thephosphorous carries over fromthe oil, and it can create prob-lems inside the diesel engine.
“A number of diesel enginesare now being outfitted with cat-alytic converters in an effort toreduce emissions. If high levelsof phosphorous are present inthe biodiesel, it can poison thecatalyst in the catalytic converterand make it unusable.”
IR spectroscopy is increasinglybeing used to test feedstock andother production components.“Biodiesel manufacturers typi-cally buy oils from several suppli-ers, and they want to assess thequality as it comes into the pro-duction plant. IR spectroscopy isa great tool for this purpose, andit can also be used to evaluatethe progress of the productionprocess,” says Armstrong.
PerkinElmer introduced itsfirst commercial gas chro-matographs more than 50 yearsago. Now it offers a family of gaschromatography instrumentation,including four biodiesel gas chro-matography turnkey systems, introduced in February 2007, to
08/07|Laboratory Equipment|11
provide a choice of high qualityanalyzers for the verification offree and total glycerin in purebiodiesel (B100) to meet ASTM(Unites States) as well as theEuropean CEN standards.
Today, PerkinElmer serves aninstalled base of some 130 to 150 biofuel labs worldwide. Thecompany maintains some 1200factory-trained and certified engi-neers, each with an average of 15 years of experience, who pro-vide predictive and preventativemaintenance, validation support,instrument repair and trainingand technical support.
Thermo Fisher Scientific pro-vides biofuel manufacturers withthe Nicolet FT-IR 380 or 6700, itsmost common base instruments.“The analytical process includestransmission, where light goesstraight through the sample byattenuated total reflection (ATR),or by using the ‘smart’ arc, whichrequires only a small sample sizefor precision and accuracy. Andthe whole analysis can take lessthan 20 seconds, a fairly highthroughput,” says Mike Bradley,Ph.D., product specialist withThermo Fisher Scientific.
He adds that IR spectroscopyis used on the production side ofbiodiesel manufacture to meas-ure raw triglyceride content infeedstock and in post processingor blending where the goal of theanalysis is to quantify the level ofbiodiesel.
Thermo also offers a GC-FT-IRcombination instrument. “Theprimary advantage is that whileFT-IRs are fast, the GC still hasthe advantage of providinggreater details by taking the ma-terial apart while the FT-IR pro-vides overall blend information,”says Bradley.
Bradley explains that some instrumentation uses calibrationsthat require dilution of thebiodiesel. “Ultimately, you needto use different calibrations fordifferent portions of the spec-trum to keep the concentrationlinear.
“With our instrumentation thiscontinued on page 12
UltraCentrifugal Millfor heavy sample loadswithout crosscontamination
ZM 200
BENEFITS:■ Heavy-duty “Powerdrive”,
speed range 6,000 - 18,000 rpm
■ Fast sample processing
■ Large surface-area sieveavoids overheating
■ Patented cassette for easysample recovery
■ Batches 10 - 4,500 ml,grind size down to40 microns
■ Versatile due to widerange of accessories
■ Easy to use, safe
BENEFITS:■ Heavy-duty “Powerdrive”,
speed range 6,000 - 18,000 rpm
■ Fast sample processing
■ Large surface-area sieveavoids overheating
■ Patented cassette for easysample recovery
■ Batches 10 - 4,500 ml,grind size down to40 microns
■ Versatile due to widerange of accessories
■ Easy to use, safe
THE STANDARD IN MANYINDUSTRIES
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continued from page 11
12|Laboratory Equipment|08/07
is not necessary,” states Bradley. “There is noneed for dilution, and one calibration frame-work may be used over the full range—all theway from 1% to 100% biodiesels.”
Another leading analytical instrumentationdeveloper and supplier is BrinkmannInstruments, a subsidiary of the Swiss-basedMetrohm AG. Larry Tucker, business develop-ment manager with Brinkmann, says thecompany offers a range of instrumentation,including the Karl Fischer line, to assess mois-ture content in biodiesel and potentiometrictitration instruments capable of assessing thequality of fatty acids in feedstock. “Titration isa quick and inexpensive way to check thequality of feedstock going into biodieselplants,” Tucker adds.
There are signs that quality service by instrument vendors is seen as a key differen-tiator in this sector. Tucker says, “We offer installation and training on our instrumentsso our customers can execute the analyticalmethods correctly.”
Younger players are also starting to make amark in this field. Aspectrics (Pleasanton,CA), which was founded in 2000, has devel-oped the encoded photometric near infrared(EP-NIR) spectroscopy technology. It recentlylaunched its multicomponent 2750 EP-NIRbiofuels analyzer, which monitors methanol,water, and total glycerin in biodiesel and water content in ethanol; performs biodieselblend determination; and analyzes ethanol/gasoline blends.
The flexible analyzer provides pass/fail information on multiple biofuel contaminantsbefore samples are sent out for ASTM certifi-cation. A single analyzer can process multiplebiodiesel and ethanol samples at 100 scansper second, generating ultra-fast, real-time results in just a few seconds.
In the next generation, more analyzers willbe dedicated to specific tasks, says Bradley.“There is a change from technical staff whounderstood every aspect of the underlyingprinciples of the tests to instrument userswho, while still technically sound are not as familiar with the versatility of some of thesystems and have to relearn them.
“Manufacturers have to ensure instrumentshave the capabilities of diagnosing them-selves—they have to work out the calibrationand the software. Plus the instruments haveto be much more intelligent and, in effect, remove the burden from a lab to diagnose and fix problems.
Bradley adds that there is much progressto report on these issues. He says the footprint of the new instrumentation is
dropping in size. “The instruments are be-coming more intelligent by indicating tooperators when they are ‘sick’ or what’swrong with them and when their calibra-tion needs updating,” states Bradley.
“While none of the instruments typicallyfound at a production laboratory setting areinordinately complex,” Shimadzu’s Jim Mottconcurs, “the proper use of this equipmentis critical to the ongoing operation andprofitability of the plant.
“Many of the users who will be tasked tooperate this equipment may be experienc-ing this level of instrumentation for thefirst time. Therefore, the success of the lab-oratory is closely tied to the ongoing sup-port of the instrumentation,” says Dr. Mott.
“Because biofuel plants tend to be locatedwhere the starting materials are located, it is common to find plants in small ruralareas, often far away from urban areas.
“Training programs must be considered a more than one-time effort; retraining andrefresher courses are critical to user satis-faction toward the instrumentation,” saysDr. Mott. •
Bernard Tulsi is a freelance writer basedin Newark, Delaware. He may be contactedat [email protected] or by phone at 302-266-6420
FFeeaattuurreedd NNeeww PPrroodduuccttcontinued from front coverprocess control can now further enhanceprocess efficiency and increase yields byanalyzing ultra-high purity gases at levelsthat previously required far more expensiveanalyzers. The HALO+ is suited to chal-lenges including fixed bulk gas continuousquality control, portable mobile analyticalcarts, process tool monitoring, air separationand gas cylinder quality control.
“The speed of response, accuracy, andpower of Cavity Ring-Down technology are nolonger the province of the elite few,” said LisaBergson, CEO of Tiger Optics. “With theHALO and the HALO+, now many morecompanies can access the great performance,low cost-of-ownership, and freedom from cali-bration high-end users have enjoyed for overhalf a decade.”
Designated as a transfer standard by manynational laboratories, and addressing over 400points worldwide, Tiger’s analyzers are basedon an absolute principle—the Beer-LambertLaw—which eliminates the need for costlyand frequent calibration. Plus, they requireno consumables, are robust and durable, andare easy to operate. •
