agilent icp-ms journal · when the hplc-icp-ms method is applied to solid samples such as tissues,...

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Inside this Issue May 2005 – Issue 23 Agilent ICP-MS Journal 2 User article: Measurement of Heavy Metals using ICP-MS for the RoHS/ELV Directives 3 Reducing Matrix Oxides with ORS 4 Analysis of Methyl Mercury in Water and Soil by HPLC-ICP-MS 5 News: ICP-MS Only Approved Multi-element Method for Drinking Waters 6 Chromium Speciation in Natural Waters by IC-ICP-MS 7 Tips & Tricks: How to Fit Your Cones Correctly, New Products for 7500 ICP-MS 8 Success Stories Contest, New-look User Forum, Up & Coming Events, Welcome to New ICP-MS Users, New Literature

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Page 1: Agilent ICP-MS Journal · When the HPLC-ICP-MS method is applied to solid samples such as tissues, soils or sediments, sample preparation is necessary. The extraction of Hg species

Inside this Issue

May 2005 – Issue 23

Agilent ICP-MS Journal

2 User article: Measurement of Heavy Metals using ICP-MS forthe RoHS/ELV Directives

3 Reducing Matrix Oxides with ORS

4 Analysis of Methyl Mercury in Water and Soil by HPLC-ICP-MS

5 News: ICP-MS Only Approved Multi-element Method for Drinking Waters

6 Chromium Speciation in Natural Waters by IC-ICP-MS

7 Tips & Tricks: How to Fit Your Cones Correctly, New Products for 7500 ICP-MS

8 Success Stories Contest, New-look User Forum, Up & ComingEvents, Welcome to New ICP-MS Users, New Literature

Page 2: Agilent ICP-MS Journal · When the HPLC-ICP-MS method is applied to solid samples such as tissues, soils or sediments, sample preparation is necessary. The extraction of Hg species

Measurement ofHeavy Metals usingICP-MS for theRoHS/ELV DirectivesNihon Environmental Services Co., Ltd.Taichi Yamamoto, Yuki Arai,Tomohiro Seki http://www.n-kankyo.com/english/english.html

IntroductionIn the EU, RoHS (the Restriction of theuse of certain Hazardous SubstancesDirective 2002/95/EC) will comeinto effect in July 2006. This directive aims at restricting the useof hazardous chemical materialsused in electric/electronic productswhile protecting the health of users ofthese products, as well as preventingenvironmental pollution that maybe caused by their disposal. ELV (TheEnd of Life Vehicles Directive 2000/53/EC) covering automotive partshas already come into force. InChina and Japan, the respectiveequivalents of the RoHS directivewill be enforced at the same time asin the EU. The Japanese version iscurrently being prepared by theMinistry of Economy, Trade andIndustry.

*Only penta and octa forms of PBDEs are restricted.

Table 1: Substances restricted by the RoHS/ELVdirectives and their thresholds

Table 1 shows the heavy metals andcompounds that are covered by theRoHS/ELV directives. In terms ofproduct manufacturing, careful controlis required to prevent the abovesubstances entering the processes,especially resin materials.Nevertheless, there has been noofficial method for analyzing metalimpurities in resin materials otherthan the BSEN1122:2001 "Plastics -determination of cadmium - Wetdecomposition method" ("EN1122")1.

Heavy MetalsNihon Environmental Services Co.,Ltd uses a 7500c ICP-MS method to

Restricted RoHS ELVsubstance directive / directive /

mg/kg mg/kgCd 100 100Pb 1000 1000Hg 1000 1000Cr6+ 1000 1000PBBs 1000 -PBDEs* 1000 -

2 Agilent ICP-MS Journal May 2005 - Issue 23 www.agilent.com/chem/icpms

analyze cadmium, lead and chromium.Quantitative determination of mercuryis also possible provided that thememory effect, the element'sadsorption to the container, and thevolatility of the material are takeninto account.

Validation of MethodsTo test the validity of their ICP-MSmethodology the lab took part inthe proficiency test in 2004(IIS04P02): "Cadmium and Lead inPlastics" that was administered bythe Institute for InterlaboratoryStudies (IIS), in the Netherlands. Atpresent, this is the only internationalproficiency test that is based on theISO/IEC Guide 43. According to thereport2, this test attracted the participation of 56 analytical institutions from 20 countries allover the world, with a large numberof participants from Japan, HongKong, China and other areas inAsia.

Three samples were used in thetest. Cadmium was the target metalfor #0454 and #0455, while lead wasthe target for #0456. All sampleswere polyvinyl chloride (PVC) moldings. Samples #0454 and #0456contained over 10 times the regulatedvalue of Cd and Pb respectively,while Sample #455 had only amoderate concentration of Cd. Theresults that Nihon EnvironmentalServices obtained were close to theaverage for both the EN1122 andEPA Method 3052 (Microwave assistedacid digestion of siliceous and organically based matrices), as shownin the example histograms for Cdand Pb in Figure 1 and 2. The calculated z-scores were within arange of ±1.

Analysts at Nihon Environmental Services Co., Ltd., Japan, in front of their Agilent 7500c ICP-MS

ConclusionThe 7500c is capable of efficientlymeasuring the 4 substances coveredby the RoHS/ELV directives as wellas the 10 heavy metals specified inthe guidelines currently preparedjointly by the industries concernedin Japan, the U.S. and the EU.3

References1. BSEN1122:2001 "Plastics - determination of

cadmium - Wet decomposition method" 2. Results Proficiency Test Cadmium and Lead in

Plastics October 20043. Guideline for Standardization of Material

Declaration by Japan Electronics and InformationTechnology Association (JEITA JGPSSI), http://home.jeita.or.jp/eps/green2.htm

Figure 2: Histogram of results for Pb in sample#0456

Figure 1: Histograms of results for Cd in sample#0454 and #0455

Page 3: Agilent ICP-MS Journal · When the HPLC-ICP-MS method is applied to solid samples such as tissues, soils or sediments, sample preparation is necessary. The extraction of Hg species

3www.agilent.com/chem/icpms Agilent ICP-MS Journal May 2005 - Issue 23

Reducing MatrixOxides with ORSBert Woods, Ed McCurdy, Don Potter,Agilent Technologies

Matrix oxides, formed when a component of the sample matrixcombines with an oxygen atom toproduce a metal oxide ion (MO+),remain some of the most troublesomeinterferences in ICP-MS. Examplesinclude CaO+ overlaps on 56Fe, 59Coand 60Ni, from the Ca isotopes atmass 40, 43 and 44 respectively, and the MoO+ interferences on all themain isotopes of Cd. Also, the oxidesof the light rare earth elements(REE's) overlap the heavy REE's.While good plasma design can reduceMO+ levels, oxide overlaps haveremained a problem, until now.Using the ORS in He collision modewith Kinetic Energy Discrimination(KED) can virtually eliminate oxidesfrom the ICP-MS mass spectrum,enabling advances in REE measurementand opening new possibilities inmaterials science applications.

Importance of Plasma DesignGood plasma and sample introductionsystem design will significantlyreduce MO+ levels by decompositionof the matrix. The parameter usuallymonitored to check plasma efficiencyis the 140Ce16O/140Ce ratio since theCe-O bond is one of the strongest M-O bonds. Decomposition of MO+

ions in the plasma is promoted by:

i) Limiting the sample aerosol loading by using a low-flow sample introduction system

ii) Removing the water vapor by cooling the spray chamber

iii) Ensuring a diffuse aerosol in theplasma, by using a plasma torchwith a wide internal diameter injector (2.5 mm)

iv) Maintaining a high plasma temperature by using a high efficiency solid-state, digital driveRF generator operating at 27.12MHz

All of these strategies are employedin the 7500 Series, resulting in atypical CeO/Ce ratio of 0.3% to 0.5%,which is 5-10 times lower thanother ICP-MS. Even at this level, oxides can still compromise analyticaldata if the parent ion is present atvery high levels compared to theinterfered ion, and especially if the

oxide bond is strong (as is the casewith REE's).

ORS/He Mode ApproachIn He mode, all polyatomic ions canbe removed simultaneously usingKED, which removes the polyatomic(molecular) ions by virtue of theirlarger size (ionic cross section),relative to the analyte ions. The largemolecular ions undergo more collisions in the cell, lose moreenergy and are filtered out at the cellexit. Efficient KED is only possibleif the ions arrive at the cell with thesame energy, and this is achievedwith the ShieldTorch System. He modehas now been applied to furtherreduce the level of oxide interferenceson the 7500ce. MO+ species are themost difficult to remove from thespectrum - however, by applying ahigher KED voltage than normal(10V compared to 4V typicallyused), and 4mL/min He to the cell,even CeO can be reduced from around 0.4% to less than 0.1%. Somesensitivity is lost, but CeO isattenuated at a greater rate than Ce.Figure 1 shows a log scale spectrumof a solution containing 100ppb Ce.Note the 140Ce16O peak at mass

156 is far smaller than the 0.186%abundant 136Ce peak. The actualCeO/Ce ratio is 0.07% - the lowest everreported for an ICP-MS operatingwith a conventional concentricnebulizer and without the use ofaerosol desolvation. Note that onlypure He cell gas was used.

Summary•He mode can virtually eliminate

CeO - x50 lower than other ICP-MS•Inert cell gas so NO new oxides,

hydrides, hydroxides or other interferences formed

•No need for desolvation devices•No interference equations used•All other analytes measured

simultaneously, in ANY matrix•Now high mass REE's can be

measured •Applies to ALL oxides and ALL

polyatomics - simultaneously

Reducing matrix oxides in this wayenables the accurate measurementof high mass REE's in natural samples without correction equationsas well as unlocking previously interfered elements in other highmatrix sample types.

Figure 1: 100ppb Ce log scale spectrum showing Ce and CeO peaks. Agilent 7500ce operated in Hemode, with normal concentric nebulizer.

Page 4: Agilent ICP-MS Journal · When the HPLC-ICP-MS method is applied to solid samples such as tissues, soils or sediments, sample preparation is necessary. The extraction of Hg species

species solution was also dilutedinto 3% NaCl (w/v in water) toobtain 100ng/L MeHg, Ethyl-Hg andHg2+. The solution was filteredthrough a 0.45um membrane beforeanalysis. A 20uL injection loop wasused for the measurement. Thechromatogram was overlaid withthe chromatogram of the purewater diluted solution at the sameconcentration, as shown in Figure 2.

The peak areas of the Hg species in3% NaCl were also integrated andthe recoveries were between 90%and 110% relative to standards inpure water. This demonstrates thatthe method is suitable for even highmatrix samples such as seawater.

Application to Soil SamplesWhen the HPLC-ICP-MS method isapplied to solid samples such as tissues, soils or sediments, samplepreparation is necessary. Theextraction of Hg species from thesolid samples is a crucial step dueto the presence of mercury in environmental samples at lowlevels, and the Hg species, especiallymethylmercury are easy to lose ortransform to other species. A simpleextraction method based on dilutehydrochloric acid was used.

The spike recoveries of the soil sampleswere between 80% and 120%.Further testing of the method andthe MeHg containing reference soilsample are planned for future work.

ConclusionHPLC-ICP-MS is appropriate forwater samples analysis, even whenthe matrix in the water sample ishigh. The method detection limits forMeHg, Ethyl-Hg and Hg2+ are betterthan 10ng/L and meet current regulatory requirements. When themethod is applied to soil samples,Hg species extraction by 7.6% HCl isappropriate, with recoveries between80% and 120%.

4 Agilent ICP-MS Journal May 2005 - Issue 23 www.agilent.com/chem/icpms

Instrumentation The aim of this work was to evaluateHPLC-ICP-MS in terms of its sensitivity and specificity for thedetermination of MeHg.An Agilent 1100 LC was coupled toan Agilent 7500a ICP-MS using the LC-ICP-MS Connection Kit(G1833-65200).

HPLC ColumnFor best results, the HPLC column(ZORBAX Eclipse XDB-C18, 2.1mmIDx50mm, 5um) should be pre-conditioned by pumping HPLCgrade methanol at 0.4mL/min formore than 2 hours, and then conditioned with eluent (same flowrate) for more than half an hour.

Results and DiscussionA series of calibration standardswas prepared from 10ng/L to100ug/L by diluting a mixed Hg speciesstock solution (1.0 ug/mL Hg forHg2+, MeHg and Ethyl-Hg, in purewater). A 20uL injection loop wasused throughout except for the10ng/L data which was obtainedusing a 100uL loop. The peak areaswere integrated for different concentration levels of 3 mixed Hgspecies.

The linear range of the calibrationcurves (Figure 1) for Hg speciationby the HPLC-ICP-MS method was at

least 4 orders. This range coversexpected real sample levels, andso the method is appropriatefor direct determination of

water samples without the application of complicatedpreconcentration procedures.

Chromatographic Separation of HgSpecies in 3% NaCl

In order to prove the abilityof the method for high matrixsample analysis, the stock Hg

Figure 1. Calibration curves for MeHg, Hg2+ and EtHg

Figure 2. Overlaid HPLC-ICP-MS ion chromatograms of 100ng/L Hg species standards in purewater (upper) and in 3%NaCl (w/v, lower) (20uL loop).

Analysis of MethylMercury in Water andSoil by HPLC-ICP-MSDengyun Chen, Agilent Technologies Co., Ltd. (China), Beijing, 100022, ChinaMiao Jing, Xiaoru WangThe First Institute of Oceanography, S.O.A,Qingdao, 266061, China

Mercury can exist either in elementalor alkylated form. Biological activitywill typically methylate mercury toeither methyl mercury or less commonly, di-methyl mercury. Thedifferent chemical forms of mercury have different toxicitieswith methylmercury species being10-100 times more toxic than inorganic mercury compounds. Asa result, the Joint FAO/WHO ExpertCommittee on Food Additives(JECFA) recently recommended theProvisional Tolerable WeeklyIntakes (PTWI) of methylmercury(MeHg) be reduced to 1.6 µg per kgbody weight per week down from3.3 µg per kg body weight per week.

The simultaneous determination ofinorganic and organic mercury isdifficult because the typical concentration of MeHg is muchlower than inorganic mercury. Themost common methods of mercuryspeciation are gas chromatography(GC) or high-performance liquidchromatography (HPLC) coupledwith a mercury-specific detector(fluorescence, photometry or otherelemental detector). The low concentration of mercury in naturalwaters leads to the need for very largesample volumes to be processed. Apre-concentration step is necessarybecause the reporting limit requiredis often below the sensitivity of thedetector used.

Page 5: Agilent ICP-MS Journal · When the HPLC-ICP-MS method is applied to solid samples such as tissues, soils or sediments, sample preparation is necessary. The extraction of Hg species

5www.agilent.com/chem/icpms Agilent ICP-MS Journal May 2005 - Issue 23

News: ICP-MS OnlyApproved Multi-element Method forDrinking WatersSteven Wilbur, Agilent Technologies Inc., USA

EPA withdraws approval of methodEPA 200.7 and SM 3120b (ICP-OES)for analysis of arsenic in drinkingwaters according to 40 CFR 141.23,effective January 23, 2006.

"These methods are inadequate fordetermining compliance, determiningeligibility for monitoring waiversand for the grandfathering of datafor the revised arsenic MCL of 10ppb (0.010 mg/L)"1. This leaves graphite furnace and hydride AA asapproved single element methods,and ICP-MS as the only approvedmulti-element method.

IntroductionIncreasing awareness of the dangersof chronic exposure to arsenic, primarily from drinking water, butalso from ingestion of contaminatedfood and inhalation of polluted air,has prompted stricter worldwideexposure regulations and monitoringrequirements. The previous maximumlevels for As in drinking water datefrom the 1950s. The World HealthOrganization (WHO) has had apublic position on As in drinkingwater since 1958 when it stated amaximum allowable concentrationof 0.2 mg/L. This was updated to0.05 mg/L in 1963. In 1993, the levelwas set to 0.01 mg/L as a provisionalguideline value, even though calculated risk of skin cancer due to

improvements in ICP-MS technologyincluding the development of extremely robust plasma conditionsto minimize suppression, and heliumcollision mode with kinetic energydiscrimination to eliminate theinterferences, permit the Agilent7500ce ICP-MS to achieve MDLs inthe range of 20 ppt (0.02 ug/L) forarsenic in typical environmentalsamples (500x lower than requiredby current regulations). Similardetection limits can be achieved inclean drinking waters using the7500a without the requirement of acollision cell. Other collision cellinstruments use complex, reactivegases or measure arsenic as a polyatomic at mass 91, both ofwhich are subject to matrix effects.

ConclusionsAfter January 2006, ICP-OES willno longer be approved for the measurement of arsenic in drinkingwater in the US. Only GFAA, hydrideAA and ICP-MS will comply. Othercountries are likely to follow suit.Of the ICP-MS solutions available,only the Agilent 7500ce ICP-MS caneffectively ionize arsenic in complexmatrices and eliminate interferencesusing simple, universal helium collision mode5. Helium collisionmode does not compromise the performance of other analytes anddoes not require matrix specificoptimizations or the use of complexor reactive gases or gas mixes.

References1. http://www.epa.gov/safewater/

ars/pdfs/regguide/ars_final_!mainguide_9-13.pdf

2. http ://www.who. int/water_sanitation_ h e a l t h / d w q / e n /arsenicun5.pdf

3. Arsenic in Drinking Water, Committee on Toxicology, Board on Environmental Studies and Toxicology, Commission on Life Sciences, National Academy Press WHO, 1993

4. EPA method 200.8, www.nemi.gov5. Trace Metals in Drinking Water

using the Agilent 7500ce ICP-MS,5989-0870EN

lifetime exposure to arsenic wasmuch lower. Practical quantificationlimits based on instrumentation atthe time precluded lower limits.2The estimated lifetime excess riskof skin cancer at the 0.01 mg/Lexposure level is 6 x 10-4 or about 1in 1700. Currently, the logistics andeconomics of treating water world-wide to meet lower levels as well asavailability of appropriately sensitivetesting methods are limiting regulationand enforcement of even lowerlevels. For a time in 2000, the USEPA proposed that the new standardbe lowered to 0.005mg/L, but thiswas later relaxed to 0.01mg/L. Infact, while the EU and US haveadopted the WHO recommendationof 0.01 mg/L, a number of countrieshave retained the 0.05 standard orsome value between 0.01 and 0.05mg/L.3 However, it is clear that the trend in permissible levels isdownward following practical limitsof quantification and that otherworldwide regulatory agencies willfollow suit, excluding the use of lesssensitive methods. Australia has, forexample, a maximum permissiblelevel of 0.007 mg/L.

ICP-MS and Arsenic MeasurementAs the need to measure arsenic atlower levels, in more complex samplesand with other elements increases,only ICP-MS will remain as a suitabletechnique. However, not all ICP-MSinstruments are equal when itcomes to arsenic measurement.Traditionally, arsenic has been oneof the "problem elements" by ICP-MS due to:

• Relatively high first ionization potential (9.81eV)

• Severe interferences from ArCl in samples containing chloride

• Mono-isotopic nature.

For relatively clean drinking watersamples, the use of mathematicalinterference correction can compensate for interferences aslong as:

1. The Cl concentration doesn't vary too much.

2. There isn't appreciable seleniumor bromine in the sample

3. A suitable internal standard is used to compensate for the matrix suppression due to its high ionization potential.

As a result of these limitations, theUSEPA reported MDLs for As byICP-MS are 1.4 ug/L4. However,

Page 6: Agilent ICP-MS Journal · When the HPLC-ICP-MS method is applied to solid samples such as tissues, soils or sediments, sample preparation is necessary. The extraction of Hg species

6 Agilent ICP-MS Journal May 2005 - Issue 23 www.agilent.com/chem/icpms

Cr column Agilent part #G3268A, 30 mm x 4.6 mm i.d

Mobile phase 5 mM EDTA (2Na), pH 7 adjust by NaOH

Flow rate 1.2 mL/min

Column temperature Ambient

Injection volume 50 ~ 500 uL

Sample prep

Reaction temp 40ºC

Incubation time 3 h

EDTA 5 ~ 15 mMconcentration pH 7 adjust

by NaOH

Table 1. Chromatographic conditions for Crspeciation

Results and DiscussionUnder the conditions describedabove, with ICP-MS detection usingthe Agilent 7500ce in H2 cell gasmode to remove the ArC and ClOHinterferences on Cr at mass 52,detection limits (DLs) of <20 ng/Lwere obtained for the individual Crspecies, as shown in Table 2.Many international regulations forhexavalent Cr specify a maximumallowable concentration of 1 µg/L,with a required DL of one-tenth ofthis level (100 ng/L), and even the smallsample volume injection of 100 µLeasily meets these requirements.However, increasing the injectionvolume to 500 µL allowed the DLsto be reduced to 13.2 ng/L forCr(III) and 15.8 ng/L for Cr(VI).

In order to test the suitability of themethod for real-world sample types, the method was applied to thedetermination of both Cr species inspiked and unspiked mineral watersamples.

Retention Time /min Peak area/counts DL (S/N=3) ng/L

Inject/uL Cr(III) Cr(VI) Cr(III) Cr(VI) Cr(III) Cr(VI)

50 0.79 2.09 1082295 914804 69.5 139.4

100 0.79 2.09 1704312 1525147 43.4 82.8

250 0.85 2.21 4939876 4546219 17.5 28.5

500 0.97 2.39 10268086 9398651 13.2 15.8

Table 2. Detection Limits for Cr Species by IC-ICP-MS

ChromiumSpeciation inNatural Waters byIC-ICP-MSTetsushi Sakai and Ed McCurdyAgilent Technologies

Measurement of total chromiumdoesn't always tell you the wholestory. The hexavalent form of theelement is toxic, while the trivalentform is an essential element forhuman nutrition. Methods to establishthe potential toxicity of Cr must therefore determine the concentrationof Cr(VI), rather than simply total Cr.

Separating and detecting Cr ischallenging because the commonforms of Cr in natural samples suchas water are chromate (CrO4

2-) forCr(VI) and chromic ion (Cr3+) forCr(III). Chromate is an anion andthe chromic ion is cationic, so asingle ion exchange method willnot work for both forms under thesame conditions. A further problemis that Cr(III) is the most stable oxidation state in samples such aswater, whereas Cr(VI) ions are strongoxidizing agents and are readilyreduced to Cr(III) in the presenceof acid or organic matter.Consequently great care must betaken during sample collection, storage and preparation, to ensurethat the Cr species distributionpresent in the original sample ismaintained up to the point of analysis.

Agilent's newly developed method

used an optimized sample stabilizationmethod, in which the samples wereincubated at 40°C with EDTA,which forms an anionic complexwith the Cr(III), allowing a singlechromatographic method to be usedto separate the Cr(III)EDTA complexand the Cr(VI).

The 7500ce ORS ICP-MS allows Crto be measured with high accuracyand good sensitivity, using the mainisotope at mass 52, by removinginterferences from ArC and ClOH.The sample preparation method,column type and chromatographicconditions used for Cr speciationare shown in Table 1.

The nonmetal IC pump (Metrohm818 IC Pump) was used to deliverthe mobile phase, but the sampleloop was filled and switched usingthe optional Integrated SampleIntroduction System (ISIS) of theAgilent 7500ce ICP-MS. While thisconfiguration maintains the highprecision and relatively high pressureof the IC pump, it provides a muchsimpler and lower cost alternativeto a complete IC or HPLC system,since only the IC pump module isrequired in addition to the ICP-MSsystem.

Na 9.1 mg/L

Ca 486.0 mg/L

Mg 84.0 mg/L

K 3.2 mg/L

Figure 1. Major element composition (mg/L) and chromatogram for spiked mineral water B.

Page 7: Agilent ICP-MS Journal · When the HPLC-ICP-MS method is applied to solid samples such as tissues, soils or sediments, sample preparation is necessary. The extraction of Hg species

7www.agilent.com/chem/icpms Agilent ICP-MS Journal May 2005 - Issue 23

Table 2. Spike recovery data for 1.0ug/L spikesof Cr(III) and Cr(VI) in mineral water B

One mineral water sample analyzedwas a French mineral water, referredto as mineral water B, which hasamong the highest levels of calciumand sulfates of any commonly availablemineral water (over 450 mg/L Caand more than 1000 mg/L sulfates).Mineral water B was analyzed withand without a spike of the two Crspecies and the spike recovery wasassessed. The results for the measuredchromatograms are shown inFigure 1, while the spike recoverydata are shown in Table 2. Themajor element composition of themineral water is shown as an insetin the chromatogram, illustratingthe very high mineral levels.Despite these high major elementlevels, the optimized sample prep.and chromatographic method gavegood chromatographic separationand identification for both Cr species.

The ability to recover low concentrationspikes for both Cr species in such ahigh matrix sample indicates theeffectiveness of the optimizedmethod for sample stabilization,which ensures that a high enoughconcentration of EDTA is availablefor complete complexation of theCr(III) species, even in the presenceof a high level of competing ions.

Furthermore the accurate recoveryof low concentration spikes of bothspecies indicates that potential problems of species interconversion(reduction of Cr(VI) to Cr(III)) wasavoided through the selection of anappropriate pH for the samples andthe mobile phase, together with theuse of EDTA in the mobile phase aswell as for sample stabilization. SeeTable 2.

Further InformationFor a full account of this applicationsee Agilent publication: IonChromatography (IC) ICP-MS forChromium Speciation in NaturalSamples, 5989-2481EN

Found (ug/L)Element Original Spike Spike Recovery

added found (%)

Cr(III) 0.05 1.0 1.10 105.0

Cr(VI) 0.24 1.0 1.27 103.0

which otherwise was left behind byacid soaking.

New Products for7500 ICP-MSAgilent have introduced two newproducts to enhance the capabilitiesof the 7500 Series ICP-MS.

Chromium Speciation Kit andMethodology (G3268A)

Separation and detection of Cr(III) and Cr(VI)at a concentration of 0.1ug/L each species

A new, simple and reliable methodhas been developed to separate andmeasure Cr (III) and Cr (VI) usingan Ion Chromatography pump(Metrohm Ltd.) coupled to anAgilent 7500ce ORS ICP-MS. For thefirst time, using the new CrSpeciation Kit, speciation of Cr (III)and Cr (VI) is possible in less than 4 minutes run time with ppt detection limits.

Strengths of the method include:

•Simple sample prep•Simple hardware •Sensitivity - ppt detection limits•Matrix tolerance - applicable to

natural waters - see previous page•Rapidity and simplicity of

methodology

New Revision of ICP-MSChemStation The new revision of ICP-MSChemStation Software (rev.B.03.02)allows Agilent GC/LC ChemStation(32bit) and ICP-MS ChemStation toco-reside on the same PC. LC/GCmethods can now be run from theICP-MS sequence table - makingspeciation studies easier and morepowerful.

Another important software development includes "Pre-emptiverinsing". The result is shortenedrinsing time and improved samplethroughput. The upgrade software(G3149B) will be available from July.See next issue of the ICP-MSJournal for more details.

Tips and Tricks:Here is a simple solution if yoursampling cone surface becomesblack - see photo below. This couldhappen if the sampling cone isn'ttightened well enough. In this casethere will be insufficient contactwith the water-cooled interface forthe heat to dissipate.

Correctly installed sampling coneafter 2 hours run with 1600 watts

Note: Do not over-tighten beyond the marked position; otherwise it may be difficult to removethe sampling cone.

User Tip from Darrel Luck, Amdel, Cardiff,Australia. A contract environmentallaboratory using a 7500c and ISISwith GE Micromist nebulizers, typicallyrunning >150 samples per day.

Amdel found that soaking the Micromist nebulizers in acids wasn'tcleaning the nebs well enough. Nowthey use a protocol of soaking thenebs over night in a mixture of 50%methanol and 50% Decon 90, a laboratory surface cleaning agent.They found the method works greatand removes the organic based contamination from inside the neb

To ensure your cones are tight enough.• Remove the sampling cone and o-

ring.• Clean the sampling cone threads.• Reattach the sampling cone (no o-

ring) to the interface. • Tighten using the sampling cone

tool. Stop tightening when the sampling cone and the cooling part of the interface are in contact. Mark the cone and the interface with a line.

• Remove the sampling cone.• Reinstall it with the o-ring in

place.• Tighten the cone until the

reference lines on the cone and interface meet.

Page 8: Agilent ICP-MS Journal · When the HPLC-ICP-MS method is applied to solid samples such as tissues, soils or sediments, sample preparation is necessary. The extraction of Hg species

New Agilent ICP-MS Users A very warm welcome to the following companies and institutions thathave recently added an Agilent ICP-MS to their analytical facilities.

• National Measurement Institute, Australia • Dept of Natl Defense,Canada • Health Canada, Canada • Taiga Environmental, Canada •Inst. Kuhlmann 2, Germany • Med. Lab. Bremen 2, Germany • Chelab 2,Italy • CTO Torino, Italy • Ingenieros Asesores, Spain • National TsingHwaUniversity (NTHU), Taiwan • Chiangmai University, Thailand • BBSRCRothamstead, UK • STL Coventry 2, UK • Capco, USA • • E-Labs 3,USA • Intel Arizona 3, USA • Molycorp, USA • San Diego State U, USA •U of Washington, USA • Underwriter Labs, USA

Share Your SuccessesContribute to the AgilentICP-MS Journal Beginning with the next issue, theAgilent ICP-MS Journal will includea regular column dedicated toCustomer Success Stories. Theseshort articles will be selected fromcontributions by customers whohave interesting stories to shareabout their success with theirAgilent ICP-MS system. Beyond thatthere are no limitations. The successcould be financial, technical, whatever.Just submit your story to our Editor,Karen Morton at [email protected] limit your draft to about atyped page, including any graphicsyou wish to include. We will takecare of proofing and final formatting,and return to you for final approval.This is a great opportunity to shareyour successes with the many regularreaders of the Agilent ICP-MSJournal.

Apple iPod Give-awayEach year, we will select what wethink is the most fascinating successstory and reprint a summary in theWinter Conference Issue of TheJournal and award the submitter anApple iPod mp-3 player. The winnerwill also receive recognition at theAgilent ICP-MS users meeting at theWinter Conference.

So get your stories in and get on thelist for the iPod. If you have any questions, contact Karen Morton [email protected] or Steve Wilburat [email protected].

Trade Shows andConferences2005 N. American Seminar Series- Agilent and MilestoneJune dates: 14 - Sacramento, 15 -Phoenix, 16 - St Louis, 21 - Montreal,22 - OttawaSeptember dates: 13 - Somerset, 14- RTP, 15 - Tampa, 20 - Vancouver,21 - CalgaryPlease visit the AgilentICP-MS website to register.

Agilent Environmental 2005Seminars31 May, Osaka, 3 June, Tokyo

This information is subject to change without notice

© Agilent Technologies, Inc. 2005Printed in the U.S.A. May 23, 20055989-2950EN

Karen Morton for Agilent Technologiese-mail: [email protected] ICP-MS Journal Editor

Agilent ICP-MS PublicationsTo view and download these latest publications, go to www.agilent.com/chem./icpms and look under "Library Information"

• Ion Chromatography (IC) ICP-MS for Chromium Speciation in Natural Samples, 5989-2481EN

• Evaluation of Conventional ICP-MS and ORS-ICP-MS for Analysis of Traditional Chinese Medicines, 5989-2570EN

• Rapid and Reliable Routine Analysis of Urine by Octopole Reaction Cell ICP-MS, 5989-2482EN

New-look Agilent ICP-MS User Forum

Many of the familiar features remain including:• e-mail notification of any activity on the Forum • powerful search facility

Additions include: • Agilent ICP-MS User Resource Library - a database specifically for

user-relevant information• "Events Calendar" - information on trade shows, conferences, seminars

and user meetings.

Because the ICP-MS User Forum is YOUR Forum we welcome your comments. Please post to the Forum, or if you prefer, e-mail Karen Mortonat [email protected] (ICP-MS User Forum Administrator).

Check out the improved ICP-MSUser Forum - the place where youcan exchange information relatingto your 4500 or 7500.

To join, you will simply need to log-into the Agilent web site, or register ifyou haven't already, and enter yourinstrument's serial number on yourfirst visit only.

Look for the link to the ICP-MS UserForum from:www.agilent.com/chem/icpms