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ICP-MS metals and Strontium Isotope Facility

Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is an analytical methodology to determine the elemental composition of liquids and solids.

ICP-MS is also suitable to determine the isotopic composition of many elements in aqueous solutions or solid aerosols produced by laser ablation. In this case, instruments equipped with several detectors (multi-collector) are needed in order to achieve the precision typically desired for isotopic ratios.

ICP-MS is one of the most sensitive analytical techniques for elements, with detection limits typically below 1 ng/kg for elements with lower ionization energies and below 1 mg/kg for elements with higher ionization energies. Because the plasma temperature is high enough to break all chemical bonds and form cations (with the exception of H, He, N, O, F and Ne,) ICP-MS provides total concentration of the elements in the sample but cannot provide information about the different chemical species containing those elements. In addition, any isobaric and polyatomic interferences are handled using collision/reaction cells or high-resolution modes which . 

Using state of the art instrumentation, the ICP-MS Metals Lab and Strontium Isotopes Lab at the Dept. of Geology and Geophysics provide analyses of trace and major elements, and heavy isotopes in a wide variety of environmental, geological, biological, engineered and forensic samples.

Agilent 8900 ICP-QQQ: Tandem quadrupole mass-spectrometer (ICP-MS/MS) with an octopole reaction system to effectively remove isobaric and polyatomic interferences. A Teledyne-CETAC MVX-7100 syringe driven autosampler capable of small (<250μL) sample sizes; quartz Scott type, PFA cyclonic and quartz double-pass spray chambers; HF introduction capable. Ni and Pt cones. Can be interfaced with laser ablation for elemental analysis of solid samples by itself or in combination with Neptune (LASS).

Thermo-Fisher Scientific Neptune Plus MC-ICP-MS: Magnetic sector mass-spectrometer with multiple collector (Faraday cups and six ion counters) for U-Pb and U-Th methods. Autosampler Elemental Scientific SC2-DX; PFA cyclonic and quartz double-pass spray chambers; platinum, nickel, or nickel jet cones; HF introduction capable. Can be interfaced with laser ablation for isotopic analysis of solid samples by itself or in combination with Agilent 8900 or additional Neptune (LASS).

Thermo-Fisher Scientific Neptune MC-ICP-MS: Magnetic sector mass-spectrometer with multiple collector (Faraday cups and one ion counters) for isotopic analysis of Sr, B, Mg, Pb, Hg, Nd, Hf, etc. Autosampler Elemental Scientific SC2-DX; PFA cyclonic and quartz double-pass spray chambers; platinum, nickel, or nickel jet cones; HF introduction capable. Can be interfaced with laser ablation for isotopic analysis of solid samples by itself or in combination with Agilent 8900 or additional Neptune (LASS).

Teledyne-Photon Machines Analyte Excite Excimer Laser Ablation system: 193nm/5ns excimer laser with fixed arm cyclonic cup for 1" mountable plugs and 25mm x 75mm x 1mm slides for analysis of solid samples on ICP-MS. Semi-quantitative spatial elemental analysis down to < 1ppm for most elements available; as well as U/Pb, Sr, and Hf isotopic analyses. Can be interfaced to several instruments for simultaneous analysis of elemental/isotopic or two different isotopic groups (Laser Ablation Split Stream (LASS).

Elemental Scientific PrepFAST MC: Automated column chemistry with specific methods available for separation and elution of pure fractions for isotopic analysis of the following elements: B, Sr

Metrohm Basic IC 883: High pressure liquid ion chromatographs for separation and characterization of both major anions (F-, Cl-, NO2-, NO3-, Br- SO42-, PO43-) and cations (Li+, Na+, NH4+, K+, Mg2+, Ca2+). Two instruments are available, each with different capabilities regarding the ion family desired. Anion-specific instrument is equipped with an ion suppressor and both are equipped with a conductivity detector.

Metrohm 905 Titrando: Automatic titrator for alkalinity measurements with pH glass electrode and 16 position autosampler.

Analytical Services

Natural Waters from Precipitation to brines, Synthetic Solutions, Aqueous Dispersions and Sludges, Nanoparticle Solutions, Protein and Cell Suspensions, etc. Typical volume required for natural water samples is 30-60 mL, see sampling details here1. Volumes required for other sample type depends on elements desired and digestion type, typically 1-10 mL.

Elemental Suite

Elements (*)

A

Li, Be, B, Na, Mg, Al, K, Ca, Sc, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Y, Mo, Ag, Cd, Sb, Te, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hg, Pb, Bi, Th, U

B

Ti, Ge, Sn, Zr, Nb, Mo, Hf, Ta, W

C

Ru, Rh, Pd, Ir, Pt, Au

D

Cl, Br, I

 

Certified Reference Materials: NIST 1643f (water), USGS AGV-1 (andesite), NIST 1515 (apple leaves), NIST 1573a (tomato leaves), NCS ZC73009 (wheat), IAEA 86 (human hair), NIES No.13 (human hair), NRC-CNRC TORT-2 (lobster hepatopancreas), NIST 1566 (oyster tissue), IAEA B5 (basalt), ERM AE120/1/3 (boric acid), USGS EN-1 (carbonate rock), NCS DC70307 (carbonate rock), NIST 2689 and1633c (coal fly ash), NIST 1641d (Hg in water), Analytika No.7004 (loam), NIST 3133 (mercury),  JSM P702-1 and P703-1 (polycarbonate), NCS 73007 (soil), NIST 86a (aluminum).

 

Total Digestion/Leaching Methods for Solid Samples, Liquid Suspensions and Organic Liquids: Hot Plate; Graphite Block and Microwave Acid Digestion (HNO3, HCl, H2SO4, HF); Ashing and Alkaline Fusion; Sequential Leaching (NH4OH, CH3COOH, HNO3, HCl, HF). 

Minerals, Glasses, Rocks, Soil and Sediments, Dust on Filters, Seston, Biological Tissues, Engineered Materials, Food, Organic Oil and Waxes, etc. Typical mass range required for homogeneous powdered samples or organic liquids is 10-250 mg.

Elemental Suite

Elements (*)

A

Li, Be, B, Na, Mg, Al, K, Ca, Sc, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Y, Mo, Ag, Cd, Sb, Te, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hg, Pb, Bi, Th, U

B

Ti, Ge, Sn, Zr, Nb, Mo, Hf, Ta, W

C

Ru, Rh, Pd, Ir, Pt, Au

D

Cl, Br, I

 

Certified Reference Materials: NIST 1643f (water), USGS AGV-1 (andesite), NIST 1515 (apple leaves), NIST 1573a (tomato leaves), NCS ZC73009 (wheat), IAEA 86 (human hair), NIES No.13 (human hair), NRC-CNRC TORT-2 (lobster hepatopancreas), NIST 1566 (oyster tissue), IAEA B5 (basalt), ERM AE120/1/3 (boric acid), USGS EN-1 (carbonate rock), NCS DC70307 (carbonate rock), NIST 2689 and 1633c (coal fly ash), NIST 1641d (Hg in water), Analytika No.7004 (loam), NIST 3133 (mercury),  JSM P702-1 and P703-1 (polycarbonate), NCS 73007 (soil), NIST 86a (aluminum).

 

Total Digestion/Leaching Methods for Solid Samples, Liquid Suspensions and Organic Liquids: Hot Plate; Graphite Block and Microwave Acid Digestion (HNO3, HCl, H2SO4, HF); Ashing and Alkaline Fusion; Sequential Leaching (NH4OH, CH3COOH, HNO3, HCl, HF). 

Mineral Grains and Rock Matrices, Volcanic Glass, Ceramics, Alloys, Thin Films, Polymers, Dry Biological Tissue, Tooth Enamel and Dentine, Bone, Otolith, Fin Ray, Keratin, etc. Petrographic slides (25x50 mm) and 25 mm diameter round mounts can be loaded in the laser ablation cell. Spot sizes between 5 and 150 mm are available. Typical detection limits for elements with low ionization potential using a spot size of 20 mm on silicates is 1 mg/g, and lower for larger spot sizes. Scanning lines on banded materials (e.g. otolith or tree rings) to determine elemental ratios is possible. Quantification of trace elements by LA-ICPMS/MS is limited by the existence of standards.
Available standards: NIST610/2/4/6 (glass), NIST 86a (aluminum); USGS MACS-3 (carbonate matrix); USGS MASS-1 (sulfide matrix), USGS BCR-2G; BHVO-2G; MPI-DING (basalt glass); IAEA B4 (tourmaline), B5 (basalt) and B6 (obsidian); In-House IsoMalt (organic matrix) and MM3 (obsidian).

 

87Sr/86Sr (Samples Introduced as Liquids): Natural Waters, Tissue, Food, Forensic, Sediment, Soil and Dust, Minerals and Rocks. Samples are purified for Sr using: 1) 50 mL manual columns with Sr-Spec resin (Eichrom) for Sr/Ca < 0.1 mmol/mol; or 2) 1 mL automatic column with SrCa resin (ESI) in PrepFAST MC for Sr/Ca > 0.1 mmol/mol. Pure Sr fractions are run in MC-ICPMS using internal standardization.
Certified Reference Materials: NIST 987 (strontium carbonate) and USGS EN-1 (carbonate rock).

 

87Sr/86Sr (Samples Introduced as Solid Aerosols by Laser Ablation): Mounted Otolith, Tooth Enamel, Mineral and Rocks with Sr/Rb > 500 g/g.
Certified Reference Materials USGS MACS-3 (calcium carbonate), In-House (marine shell and synthetic apatite).

 

208Pb/204Pb, 207Pb/204Pb, 206Pb/204Pb (Samples Introduced as Liquids): Tissue, Food, Forensic, Sediment, Soil and Dust, Minerals and Rocks. Samples are purified for Pb using 50 mL manual columns with Sr-Pb-Spec resin (Eichrom). Pure Pb fractions are run in MC-ICPMS using internal standardization (thallium).
Certified Reference Materials: NIST 981(lead) and NIST 997 (thallium).

 

 δ11B (Samples Introduced as Liquids): Natural Waters with [B] > 20 mg/kg, carbonate rock with [B] > 10 mg/kg. Samples are purified for B using 50 mL 1 mL automatic column with Amberlite IRA743 resin in PrepFAST MC.  Pure B fractions are run in MC-ICPMS using standard bracketing with in-house B isotopic standard.
Certified Reference Materials: NIST 951a (boric acid), IAEA B1 (sea water), IAEA B2 and B3 (ground water), ERM AE 120, 121 and 122 (boric acid). 

 

LA-U-Pb-trace elements: Zircon, titanite and monazite mounted grains can be analyzed using ICP-MS/MS, MC-ICPMS or SS (LA-MC-ICPMS + LA-ICP-MS/MS).
Standards: 91500, PL, Plesovice, Temora II, Mudtank, R33, MKED, Monazite.

 

U-Th (Carbonate Rock): Carbonates with [U] > 25 mg/kg and U/Th > 10 g/g. Samples are spiked with 233U-236U-229Th and purified for U and Th using 1 mL manual columns with resin Aix-8.  Pure U and Th fractions are run in MC-ICPMS using standard bracketing in-house standard calibrated against HU1 and CRM 145.
Certified Reference Materials:  NBNL CRM145 (Natural Uranium).

 

Anion and Cation Chromatography: Filtered, non-acidified, oxygenated water samples with TDS (total dissolved solids) below 500 parts per million for straight analysis. Higher TDS samples such as brine dilutes gravimetrically with Type I water. Typical volume required for natural water samples is 30 mL, see sampling details here1.

 

Alkalinity: Filtered, non-acidified, natural water samples are titrated with an automated instrument to a set pH in order to determine the buffering capacity of the sample. Typical volume required for natural water samples is 100 mL, see sampling details here1.

 


Sample Handling

 

Elemental analyses for both filtered (“soluble”) and raw (“total recoverable”) water and wastewater samples  following U.S. EPA 200.8 (Determination of Trace Elements in Waters and Wastes by Inductively Coupled Plasma-Mass Spectrometry) are available. Collecting water samples for the determination of the “soluble” fraction of trace elements require strict protocols:

Containers to collect samples: Use low density polyethylene (LDPE) bottles >30 mL, acid leached in 10 % HCl at 65o C, rinsed with Type I water and dried in a dust-free environment like a laminar flow bench, individually Ziplock bagged. In some cases, it is possible to use acid leached 5-10 mL polypropylene (PP) centrifuge tubes to keep samples. For a detailed acid leaching protocol go here(2).

Filter: acid leached with 10 % HCl and rinsed with Type I water, 0.45 mm cartridge filter with polyethylene with Luerlock connector and 50 mL polypropylene syringe.

Auxiliary bottle to load syringe: 125-500 mL acid leached LDPE wide mouth bottle.

 

Clean Hands – Dirty Hands protocol:

Dirty hands: rinse auxiliary bottle with sample to be collected a few times, fill it and cap it. Let particles to settle for one minute and excess water on the outside of bottle and threads to drain. When clean hands are ready, pour carefully from auxiliary bottle into syringe (filter cartridge on) held by clean hands. Auxiliary bottle can be reused provided the conductivity of different samples is similar or when the samples are taken in order of increasing conductivity.

Clean hands: Prepare a clean surface to work (like a cooler top or small table). Open large Ziplock bag containing individually bagged sampling kits and put it on clean surface.  Put non-powder gloves on (vinyl or nitrile) and take one sampling kit. Remove sample bottle from Ziplock bag, open sample bottle and leave bottle and cap in Ziplock bag. Remove syringe and filter cartridge from Ziplock bag, remove plunger and screw filter in syringe. Hold syringe for dirty hands to fill it carefully to about 75% of syringe volume from auxiliary bottle. Replace syringe plunger and filter into sample bottle. Discard the first 5 mL to remove any liquid left from filter cleaning. Discard syringe with filter cartridge, close sample bottle tightly and place back in Ziploc bag. Put bagged sample in a second large Ziplock bag containing samples. 

 

Storage and acidification: keep sample in cooler with ice and acidify with > 0.3 mL of concentrated HNO3 or HCl (trace metal grade) within 24 hs. 

 

Water Sample Volumes required

Minimum Sample Volume (mL)

Conductivity (mS/cm)

Conditions

 

<500

500-10000

>5000

 

Trace elements by ICPMS

125

30-60

5-10

Filtered or Raw, acidified to pH < 2 with HCl (trace metal grade)

Major ions (ICA + ICC)

30

30

10

Filtered, not acidified

Alkalinity

125

125

125

Filtered, not acidified

 

Sampling kits including acid leached polypropylene 15 mL centrifuge tube, or low-density polyethylene narrow mouth 30-125 mL bottle, syringe and cartridge filter can be provided. Sampling tubes or bottles may have acid in the for sample preservation.

Prepare 10% HCl (v/v, AR grade) in a large plastic capped container (ideally a carboy with spigot) and fill bottles or tubes (not used) leaving ~10% volume headspace. Fill a Ziplock bag with one or two full layers of bottles or tubes, depending on their size. Do no mix different sizes in the same bag. Place bag in oven at 65o C in a Pyrex tray, stacking bags flat on top of each other. Leave for one day, then turn over the bags and leave them for a second day. Remove from oven and let bottles cool down to room temperature, then pour the acid contained in bottles or tubes back in the 10% HCl container (carboy). Rinse bottles or tubes individually and thoroughly (outside and inside) using Type I water. After rinse, fill the bottle or tubes with Type I water, cap them and put them in a clean plastic box. Take the box with containers into laminar flow and let the outside of containers to dry. Open containers one by one, empty the water gently into waste plastic container placed inside laminar flow bench and let them is dry on racks. Cap containers and Ziplock bag clean dry bottles or tubes. Store in in designated clean drawers. 

 

Elemental Suite

Elements (*)

A

Li, Be, B, Na, Mg, Al, K, Ca, Sc, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Y, Mo, Ag, Cd, Sb, Te, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hg, Pb, Bi, Th, U

B

Ti, Ge, Sn, Zr, Nb, Mo, Hf, Ta, W

C

Ru, Rh, Pd, Ir, Pt, Au

D

Cl, Br, I

 


 

Method Unita Internalb Notes
Elemental suite A sample $22-$94 1,2,4
Elemental suite B sample $36-$60 1,3,4
Elemental suite C sample $36-$51 1,3,4
Elemental suite D sample $36-$42 1,3,4
Silicon sample $22 1
Phosphorous sample $22 1
Sulfur sample $22 1
ICP-MS/MS (solution) hour $50 1
MC-ICP-MS (solution) hour $95 1
LA-ICP-MS/MS hour $85 5
LA-MC-ICP-MS hour $130 5
LA-SS hour $180 5
87Sr/86Sr (solution) sample $75 1
δ11B (water) sample $125 1
208Pb/204Pb, 207Pb/204Pb, 206Pb/204Pb sample $125 1
LA-ICP-MS/MS-U-Pb DZ (N=300/600) sample $550/$850 5
LA-MC-ICP-MS/MS-U-Pb DZ (N=300/600) sample $850/$1300 5
U-Th (carbonate) sample $250 6
ICA sample $10 1,8
ICC sample $10 1,8
Alkalinity sample $10 1
Sample prep/Digestion hour $100 7
Water Sampling kit $15 9

Notes

Assisted hourly rate: 100%

External charges: Academic Institutions and Government Agencies 50%; Private companies 100%.

  1. Extra charges for filtering of liquid samples and grinding, leaching and digestion of solid or organic samples
  2. First element charge $22, each extra element $1.5
  3. First element charge $36, each extra element $3
  4. When major and trace elements are present in the same suite, they are charged as two separate suites
  5. Extra charges for mounting solid samples
  6. Concentration 100 ng U/g of CaCO3; 238U/232Th > 10 g/g
  7. Volumetric and gravimetric dilution, filtering, grinding, leaching, acid digestion, ashing and alkaline fusion range between $2-$50 per sample.
  8. Extra charge for dilution of brines
  9. Kit contains acid-leached LDPE bottles (30-125 mL), syringe and cartridge filter in individual Ziplock bags.

Solid and liquid samples can be shipped to:

Diego P Fernandez
115 So. 1460 E, Rm 383
Dept. Geology and Geophysics
Salt Lake City, UT 84112
 

Please send an email to diego.fernandez@utah.edu including tracking number, and the submission form linked below filled out and signed.

As of 8/23/2020, due to security and health concerns please contact us prior to shipping or delivering samples.

Document Sample Submission Form

Last Updated: 9/21/20