Inside this Issue November 2009 – Issue 40 Agilent ICP-MS Journal 2 Manufacturing Step-up to Satisfy Strong Early Sales of 7700 Series ICP-MS 3 Success Story: Accurate Results from 7500 Series ICP-MS Shortens Time to Lab Accreditation 4-5 Characterization of Nanoparticulates using Field Flow Fractionation-ICP-MS 6 IDEA™ Achieves Definitive Accuracy without Calibration Curves 7 Well Equipped ICP-MS User Training Lab Opens in Americas 8 Two Free Webinars on Improving Data Quality in ICP-MS, 7700 Seminars and User Group Meetings, Conferences and Trade Shows, Winter Plasma Conference 2010
Transcript
Inside this Issue
November 2009 – Issue 40
Agilent ICP-MS Journal
2 Manufacturing Step-up to Satisfy Strong Early Sales of 7700 Series ICP-MS
3 Success Story: Accurate Results from 7500 Series ICP-MS Shortens Time to Lab Accreditation
4-5 Characterization of Nanoparticulates using Field Flow Fractionation-ICP-MS
6 IDEA™ Achieves Definitive Accuracy without Calibration Curves
7 Well Equipped ICP-MS User Training Lab Opens in Americas
8 Two Free Webinars on Improving Data Quality in ICP-MS, 7700 Seminars and User Group Meetings, Conferences and Trade Shows, Winter Plasma Conference 2010
2 Agilent ICP-MS Journal November 2009 - Issue 40 www.agilent.com/chem/icpms
Manufacturing Step-up to MeetStrong Early Ordersof 7700 Series ICP-MSDon PotterWorldwide ICP-MS Marketing Manager,Agilent Technologies, Santa Clara, CA, USA
Since its introduction in July 2009,the 7700 Series has generated agreat deal of interest and has enjoyedunprecedented demand: over 140orders have been placed for the 7700Series between July and October. Inaddition, a number of 7500 Seriesorders have also been placed to fulfill existing purchase contracts.
Building on the market leadership ofthe 7500 Series, the rapid acceptanceof the 7700 Series confirms that high performance combined withruggedness and ease of use are themost important requirements forICP-MS buyers.
To satisfy the strong demand for the7700, the ICP-MS manufacturingteam is working at near-full capacityin their state-of-the art productionand test facilities at Agilent’s TokyoAnalytical Division (TAD) in Japan(Figure 1).
Milestone reached: First shipmentof 7700 ICP-MS leaves TokyoThe TAD team took some time out inlate July to celebrate the shipment ofthe first 7700 ICP-MS unit destinedfor a customer lab (Figure 2).
The 7700s mainframe shown was onits way to support the developmentof new pharmaceuticals at ScheringPlough Research Institute (SPRI) inUnion, New Jersey, USA.
Figure 1. Agilent 7700 (and final 7500) Series ICP-MS assembly and final test facility in Tokyo, Japan
Figure 2. Agilent’s Tokyo based ICP-MS team celebrate the shipment of the first 7700 ICP-MS toSchering Plough Research Institute (SPRI) in the U.S.
www.agilent.com/chem/icpms 3Agilent ICP-MS Journal November 2009 - Issue 40
Success Story:Accurate Results from7500 Series ICP-MSShortens Time to LabAccreditationEnvirolab Services, Sydney, Australia
Accreditation signifies that an environmental testing lab can produceprecise, reliable results for its clients –and is often a prerequisite for generating revenue. The managementteam at Envirolab Services wasdelighted when they required onlytwo months to gain full accreditationfor analyses on their new Agilent7500 Series ICP-MS – a rare feat thateven the assessor considered impossible prior to his visit. With anOctopole Reaction System (ORS)that removes molecular interferences(that might compromise reportinglimits for key elements), the instrumentcontinues to deliver accurate resultsand helps the lab to expand itsbusiness.
The CompanyEnvirolab Services is a high-techscientific laboratory that serves theenvironmental sector. Although thelab was founded by ManagingDirector Tania Notaras only fouryears ago, it has rapidly grown toabout 40 employees and is now amajor supplier of environmentalanalytical services in New SouthWales. The lab runs thousands ofsamples per month in its two-storysuburban premises, a facility purpose-built to world class standards in2008.
In-house ICP-MS for BetterCustomer ServiceEnvirolab Services originally usedICP-OES and AA instruments forless demanding analyses. But threeyears ago, when customers neededresults for trace-level metals, the labwas forced to send out samples to athird party for analysis using themore sensitive ICP-MS technique.Turn-around times were long, andeventually the team at Envirolabdecided to purchase an in-houseICP-MS to provide better service toclients.
Giovanni Agosti, the lab’s highlyexperienced Technical Development Manager, explained that they chose
Growing BusinessNotaras and Agosti described howthe 7500ce has allowed them to takeon new types of work related tolandfills and groundwater, whichhas increased their revenue in bothICP-MS and other analyses. “We’rerunning a lot more samples now, sothe instrument is paying itself off. Wehave been able to build up our businesswith this instrument,” said Notaras.
When asked if there were any surpriseswith the instrument, Agosti replied,“I have been positively surprised athow well the collision cell works. Wecan now accurately analyze arsenicand selenium at low levels in complexmatrices.”
Notaras added, “We often get betterresults than our competitors. Someclients want to compare, so theysplit samples. Because of the ORS,we always come out ahead.”
Further InformationVisit Envirolab Services’ web site at:www.envirolabservices.com.au
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the Agilent 7500ce ICP-MS after sending a wide range of difficult testsamples to a number of vendors.Agilent provided the best results.Notaras commented that “In makingthe choice, we also looked atrobustness and reliability, and considered the good relationship wehave with Agilent. From day one,Agilent has always looked after us.”
Rapid AccreditationThe lab quickly achieved accreditationfrom the Australian-based and internationally recognized NationalAssociation of Testing Authorities(NATA). Agosti remarked, “After theinstrument was installed, we wereable to get trained and complete validation of all our methods inabout two months. That was a greatachievement for us. We ran almost1000 samples during the validationperiod. Gaining accreditation in twomonths meant we were able to runpaying samples in a very short time.”
Notaras added, “Two months is veryquick. The assessor came out butwas not planning to give his signatureto the accreditation. He did notthink it possible to train and validatein only two months. He was pleasantlysurprised by our technical expertiseand the validation results, andimmediately granted accreditationwith no restrictions. That is veryrare.”
More Accurate Results for Difficult SamplesSeawater is one of Envirolab’s mostchallenging matrices for ICP-MS analysis for trace metals, in partbecause it produces polyatomicinterferences for metals like arsenicand selenium. The Agilent 7500 SeriesICP-MS systems are designed toaccurately measure low levels ofthese metals in high-matrix samples.The unique ORS is a highly efficientcollision/reaction cell (CRC) thatremoves the majority of polyatomicinterferences.
Agosti explained that he had usedICP-MS instruments previously, butthe Agilent system was the firstexperience he had with a collisioncell. When asked if he thought the ORSimproved the analysis of difficult elements/sample matrices, he exclaimed, “Definitely! This instrumentis quite amazing. After all the validationusing real samples, I know theresults I’m getting in the end are theright results. I am confident in thisinstrument.”
Giovanni Agosti with the Agilent 7500ce ICP-MS .
4 Agilent ICP-MS Journal November 2009 - Issue 40 www.agilent.com/chem/icpms
Figure 1. Fractograms of GSL deep brine water sample (site 3510 at 7.5 m in depth; sample collected on 10/26/07). Size range: 0.9 - 7.5 nm.
phases containing major and traceelements. The flow of higher densitywater (1160 kg/m3) from the northarm to the less dense south arm(1100 kg/m3), yields a persistentlayered system with an oxic brineupper layer and an anoxic brine deeper layer, yielding strongly contrasting geochemical conditionsover a 9 m vertical distance.
The GSL hosts a large avian populationthat is potentially affected by tracemetals and metalloids such as Se, Asand Hg, and natural nanoparticulatesmay act as a gateway for introducingtrace elements into the food chain ofthe lake. Laboratory experiments haveproven that mineral nanoparticles maybe directly ingested by mixotrophicphytoplankton, which constitute thebase of the GSL food chain.
This work examines the size distributionand elemental composition of nano-particles from oxic and anoxic samples in the GSL, with the workinghypothesis that the size and elemental
Characterization ofNanoparticulatesusing Field FlowFractionation-ICP-MSXimena Diaz, William P. Johnson,Diego Fernandez, David L. Naftz Depart. of Geology & Geophysics, University of Utah, Salt Lake City, USA
IntroductionRecent interest in the analysis ofnanoparticulates in the environmenthas largely centered on the potentialimpacts of manmade particles.However, natural nanoparticles areubiquitous in aquatic environments.The Great Salt Lake (GSL) is a usefulfield laboratory in which to testmethods for analysis of nanoparticles.Being a hypersaline terminal lake,the GSL has high concentrations ofdissolved solids and it is super-saturated with respect to many
distributions differ strongly amongthe oxic and anoxic layers.
MethodsFlow-field flow fractionation (FIFFF)is a minimally invasive techniquethat uses hydrodynamic principles anda thin rectangular channel to separateparticles by size. Asymmetric flow-field flow fractionation (AF4) uses atrapezoidal channel which reducessample dilution relative to symmetricchannels and provides exceptionalnanoparticle size resolution. Todetermine the trace elemental distribution in fractionated particulates, the AF4 was coupledwith an Agilent 7500ce ICP-MS withan Octopole Reaction System (ORS)cell. The 7500ce was calibrated usinga mixed standard (plus 1 mg/L Csinternal standard) added to the AF4carrier solution. Adding an internalstandard to the carrier rather thanthe sample avoids discrepancies dueto variations in solution flow to thedetector during fractionation. Toincrease the sensitivity of trace
elements such as Se and As, methanolwas added to the carrier solution(3% v:v). A total of 16 elements (Al,Mn, Fe, Co, Ni, Cu, Zn, As, Se, Mo, Sb,Au, Hg, Pb, U, Cs) were measured byAF4-ICP-MS.
ResultsTrace elements such as Mn, Pb, Zn,Cu, U, Ni and Co were associatedwith nanoparticles in the 1 - 2 nmsize range (Figure 1, blue and greenrectangles), as well as the 5 - 7.5 nmsize range (Figure 1, red rectangles).These nanoparticle size fractionsand elemental associations with Mn,Pb, Zn, Cu, U, Ni and Co were observedin the deep brine sample (Figure 1),but also in the shallow brine. Figure 1shows a continuum in signal intensitiesfor these elements, increasing withincreasing depth (increasing degreeof O2 depletion and sulfide presence),suggesting the formation of sulfides.Aluminum showed a peak only in the5 - 7.5 nm size range (not in the 1 - 2nm size range) with this peak beingsomewhat larger in the deep brinesamples relative to the shallow brinesamples (Figure 1). Mercury was significant in the 1 - 2 nm size in theanoxic deep brine sample (Figure 1),but was not present in the shallowbrine samples. In contrast, arsenicwas present in the 1 - 2 nm size range,but was most significant at shallowdepth and much less significant indeeper samples. It should be notedthat the raw signal intensities inFigure 1 are not corrected for influences of ionization efficiency;these influences are corrected in theintegrated elemental masses describedbelow.
Figure 2 shows concentrations (perL solution) of particulate-associatedelements as a function of depth andsize range. For >450 nm microparticles,the concentrations of nearly all associated elements increased withdepth (Fig. 2 top). The same observation held for the 10 – 250 nmnanoparticles (except Co, As, andSb) (Fig. 2 middle). In contrast to the>10 nm size range, the majority ofthe trace element concentrations inthe 0.9 - 7.5 nm size range did notincrease with depth (Fig. 2 bottom),except for Al, Mo and Hg. The majorityof trace element mass associatedwith particulates was in the >450nm size range, as shown by comparingthe measured concentrations (per Lsolution) between the 3 particulatesize ranges (Figure 2). The trace element mass associated with the 10- 250 nm size range was much lower(multiple orders of magnitude for
tool for determining the trace elementalcomposition of nanoparticulates incomplex aqueous environments.Associating nanoparticle size fractionsand elemental composition betweenthe shallow oxic and deep anoxicbrine layers of the Great Salt Lake isexpected to help understand thepathways of toxic and other elementsinto the food chain.
some elements) relative to the > 450nm size range. The same was true forthe 0.9 - 7.5 nm size range, but withgreater concentrations of Ni, Zn, Auand Pb in the 0.9 - 7.5 nm size rangerelative to the 10 – 250 nm sizerange.
ConclusionsThe results demonstrate that AF4-ICP-MS with ORS is a simple but powerful
5www.agilent.com/chem/icpms Agilent ICP-MS Journal November 2009 - Issue 40
Figure 2. Concentration of trace elements for site 3510 at 0.2 m, 3.0, 6.5 and 7.5 m in depth. Top: size range>450 nm. Middle: size range between 10 - 250 nm. Bottom: size range between 0.9 – 7.5 nm.
6 Agilent ICP-MS Journal November 2009 - Issue 40
refining process, thus maximizingprofits.
The same method and 3Hg-SPC Kit isutilized by Centers for Disease Controlto accurately test blood samples forhigh-priority industrial metals. Amongthese, accurate speciation of Hg is acritical requirement (Figure 2).
The problems for which IDEA metrology is providing solutionsrange from environmental monitoringto biochemi-marker™ discovery andquantitative measurements in biological samples. Biochemi-markerswill soon help physicians confirmdiagnoses of diseases earlier andmore accurately. With IDEA (Figure 3),scientists are generating previouslyunavailable information about diseasessuch as autism and cancer.
IDEA, CCFQ, i-Spike, SPC and biochemi-marker are trademarks ofApplied Isotope Technologies, Inc.
Example of capabilities of IsotopeDilution Enabled Automation (IDEA)with ICP-MS in environmentalhealth and industrial monitoring.
During the past 5-6 decades, therehad been many advances in IsotopeDilution Mass Spectrometry. Its wideracceptance for routine use, however,has been hindered by technical complexities, especially for accuratemulti-species analysis. One group ofenabling metrologies and tools called Isotope Dilution EnabledAutomation overcomes many ofthese obstacles.
The IDEA-MS concept includes aunique Calibration Curve FreeQuantitation (CCFQ™*) packageincorporating a mathematical foundation that utilizes additionaldegrees of freedom to achieve unprecedented accuracy, multi-analyte,multi-species capability and shorter,simplified application. The CCFQsoftware also includes a Spike-to-Analyte optimization tool that allowsthe user to select the appropriateerror propagation factor and corresponding amount of spike tohelp deliver or maintain the desiredlevel of accuracy for each element.For sample processing, the key automation tool is the i-Spike™ sorbent-cartridge that is used for
Figure 1. The Hg-SPC Kit is capable of 4 differentMethod 6800 compliant measurements and 9inter-species conversion values. This work wasdone with an Agilent GC-ICP-MS (ref:Spectroscopy January 2010).
*CCFQ-SIDMS algorithm is described in the EPAMethod 6800 document: http://www.epa.gov/waste/hazard/testmethods/sw846/pdfs/6800.pdf
in-flow spiking and equilibration,facilitating rapid analytical cycles toaddress the demands of high-through-put workflows.
CCFQ-SIDMS is now accepted worldwide as the most accuratemetrology for delivering definitiveand legally-defensible multi-speciesresults. Recognizing the utility ofIDMS/SIDMS, the US EPA haspublished them, after global scientificscrutiny and stellar performance, asa national Resource Conservationand Recovery Act (RCRA) method,Method 6800, which is dedicated tothe ID metrology. Method 6800 isnow accepted as the gold standardfor speciation.
AIT’s 3Hg-SPC™ Kit, for example,enables simultaneous definitivemeasurement of 3 mercury species,while using the same extracted sample for Non-Extractable (NE) Hg,including metallic mercury (Hg0). Inthe near future, AIT will expand themethod to include Hg-species amongthe NE group (Figure1). This particularapplication is ofgreat interest to oilrefiners becauseaccurate Hg-speciesinformation enablesprocess optimizationto minimize catalystpoisoning in the
*NE-Hg: Non-Extractable Mercury, including Hg0
Figure 2. CCFQ-based, simultaneous 3 mercury species analysis using AIT’s 3Hg-SPC Kit. Optimized GCconditions and Method 6800 implementation minimized formation of metallic Hg and helped achieve pptlevel quantitation for 3 species simultaneously. Courtesy of Prof. Kingston and Dr. M. Rahman, DuquesneUniversity, Pittsburgh, PA.
Figure 3. Advanced IDEA metrology and CCFQ significantly improves accuracy of species measurement by eliminating or minimizing biases from a variety of sources.
Expert Team of TrainersThe team of course leaders combinetraining and development experiencewith many years hands-on operationof ICP-MS systems in different industries. With nearly 20 yearsdirect experience with ICP-MS, TomRettberg’s areas of applications specialization include EPA environmental analysis, high puritysemicon materials analysis, solidsample analysis, organic materialsanalysis, isotope and earth scienceapplications. Thong Quang Ta has beendelivering applications support, consulting, and training for AgilentICP-MS in North America since 2005with previous experience in thesemiconductor, environmental andclinical applications. Philip Schmidt,who created the training facility,brings specialized applications experience from silicon wafer
Well Equipped ICP-MSUser Training LabOpens in Americas Lisa Trainor ICP-MS Sales and Support, USA
Opened in Sept 2009, the ICP-MSTraining Facility was established toprovide a new approach to ICP-MStraining for analysts who are eithernew to the technique, unfamiliarwith the Agilent system or whorequire additional training.
Training for Analysts Based in theAmericas and BeyondLocated in the historic district of StCharles in Missouri, USA, the ICP-MS Training Facility is only 16km (10 miles) from St Louis’International Airport. With sucheasy communication links, analystsfrom outside of the Americas arewelcome to join any of the range oftraining courses. Currently, there are5 different ICP-MS training coursesoffered at the ICP-MS TrainingFacility.
New Teaching Approach EnhancesLearningThe advanced training facilities havebeen carefully designed so that thetwo Agilent 7500 ICP-MS systemsand attendee desks and seating arelocated in the same room (Figure 1).Use is also made of two 100 in. screensthat are used to deliver trainingmaterials and to relay the ICP-MSsoftware suite. Wireless keyboardsare also utilized to give students thechance to operate the ICP-MS fromtheir seats. And with a maximum of10 students per course, everyone issure to have ample occasion forhands-on learning and the time toask the course-leader about specificpoints. Feedback from the inauguralcourse, led by Dr. Tom Rettburg, wasoverwhelmingly positive (Figure 2).
Course Title Duration/days
7500 ChemStation 4
7500 MassHunter 4
Spanish ICP-MS Training Course 4
Advanced ICP-MSTuning and Maintenance 3
Environmental Applications 3
manufacturing together with general knowledge built up over 8 years asan Applications Engineer. The founderof the ICP-MS Training Facility andICP-MS expert, Abe Gutierrez, leadsclasses in Spanish.
To find out more on the courses heldat the ICP-MS Training Facility,contact Lisa Trainor:[email protected] or tel: US972-977-4684
7www.agilent.com/chem/icpms Agilent ICP-MS Journal November 2009 - Issue 40
Figure 1. Combining laboratory and lecture facilities in cutting edge training premises specifically for Agilent 7500 ICP-MS users.
Figure 2. Participants of the first training course held at the Agilent Training Facility in September 2009. Trainer Dr TomRettberg is on the right of the photo.
ICP-MS, thereby making such qualifier ions available for evaluation of dataquality.
In the second Webinar, they will present data demonstrating the use of qualifier ions to improve ICP-MS data quality in complex sample matrices, byconfirming the measured result from the primary isotopes.
Title: Part 1: He Mode Interference Removal for Spectral Clarity andMulti-Isotope Confirmation
Date: Wed, December 16, 2009Time: 08:00 PT (USA)
11:00 ET (USA)16:00 GMT (UK)17:00 CET (Central Europe)
Part 2: Using Qualifier Isotopes to Validate Multi-Element ICP-MS Data in Complex Sample Matrices
Date: Wed, February 10, 2010Time: 08:00 PT (USA)
11:00 ET (USA)16:00 GMT (UK)17:00 CET (Central Europe)
To register go towww.spectroscopynow.com and look for the “Webinars” link.
You will then need to click on the Agilent Technologies entry.
Or use the direct link:www.spectroscopynow.com/coi/cda/detail.cda?id=22519&type=Feature&chId=1&page=1
Front page photo: Arun Kumar Raju and Ramesh Muthukumarasamy,Agilent ICP-MS Application Chemists based in India
Two Free Webinars on Improving Data Qualityin ICP-MS
7700 Seminars andUser Group MeetingsAgilent has an on-going program of7700 Series ICP-MS seminars andUser Group Meetings. Be sure tocheck with your local Agilent officeor www.agilent.com/chem/eventsweb page for details of events in yourarea. Example events include:
Agilent Environmental Seminars, Jan 19 and 21, 2010, SpainICP-MS User Meeting, Jan 27-28,2010, FinlandICP-MS User Meeting, Feb 11, 2010,Denmark
Pittcon 2010Feb 28 – March 5, 2010Orlando, USAwww.pittcon.org
Agilent Events atWPC 2010Date for your diary:Tuesday Night Agilent ICP-MS User Meeting &ReceptionJanuary 5, 2010, Calooza Ballroom18:30 - 21:30
All Agilent ICP-MS users attendingthe 2010 Winter Plasma Conferenceare invited to join Agilent’s ICP-MSUser Meeting.
This popular event offers you theopportunity to find out about thelatest developments in ICP-MS aswell as interact with Agilent's teamof ICP-MS experts and fellow users.With limited places, users mustregister to get a ticket, to be pickedup at the Agilent booth onMon/Tues. Register online now at:www.agilent.com/chem/wpc
Agilent Events atWPC 2010
This information is subject to change without notice.
Karen Morton for Agilent Technologiese-mail: [email protected] ICP-MS Journal Editor
Agilent’s Ed McCurdy, ICP-MS ProductMarketing, and Steve Wilbur, ICP-MSEnvironmental Marketing, willexplore the capability of the 7700xORS3 helium (He) mode to removethe polyatomic interferences fromall isotopes of the target elements, so allowing the user tomeasure additional isotopes formany analytes. This approach is widelyused in organic mass spectrometry,where these secondary ions arereferred to as "qualifier" ions.
In the first Webinar of this series, Edand Steve will assess the fundamentalperformance of He mode in removing spectral interferences in
