Earth Sciences Division (ESD) Department of Energy (DOE) Lawrence Berkeley National Laboratory (LBNL)



Aqueous Geochemistry Lab (ESD-AGL)

The Earth Sciences Division's Aqueous Geochemistry Lab (AGL) is a research lab specializing in aqueous geochemical/biochemical studies. The lab has a modest selection of analytical instruments as well as experimental equipment to support its research projects. The analytical instruments are also available for other projects and users within LBNL (you need to have an LBNL chargeable account).

The new Aqueous Geochemistry Analytical Service Center has been set up within the Earth Sciences Division at Lawrence Berkeley National Laboratory effective October 1, 2012 to provide ICP-MS (Inductively Coupled Plasma-Mass Spectrometry) elemental analyses of aqueous samples.  With the optional use of microwave digestion available in the Center, it is also possible to determine quantitatively elemental abundances of solid samples.  Speciation of selected elements (e.g., selenium, arsenic, chromium) can be carried out using the dedicated High Performance Liquid Chromatography (HPLC) instrumentation.  Analyses ranging from Semi-Quantitative (72 elements) to Ultra-Trace Metal analysis are available.  Analyses can be run on a sample by sample fee basis by the staff in the Center, or time can be rented on the instrument for self-analysis.  A detailed list of services and fees is available in PDF format here.

Analytical Equipment

  1. Perkin Elmer SCIEX Elan DRC II Inductively Coupled Plasma Mass Spectrometer. This is a quadrupole mass spectrometer with a dynamic reaction cell (DRC). It can be used for concentration measurements, isotope ratio, isotope dilution and isotope abundance analysis. 
  2. Perkin Elmer 200 series HPLC system with autosampler, quarternary pump, column oven and a vacuum degasser. Samples collected in special gas/atmosphere environment can be sampled from capped vials. The HPLC can be used with a UV detector - or interfaced with our ICP-MS for speciation of metals.
  3. Dionex ICS-2100 Integrated Reagent-Free IC system for anion and cation analysis
  4. Shimadzu TOC-VCSH high sensitivity inorganic/organic carbon analyzer with a wide range analytical capability from 4 ug/L to 25,000 mg/L carbon. The unit is also equipped with a SSM-5000A module for solid sample analysis and an ASI-V autosampler for aqueous samples.
  5. Computer controlled Mettler DL50 Graphix auto titrator with LabX software and auto sampler for fully automated analysis. It is currently set up for low alkalinity measurements in small samples (~1 mL), and runs both Inflection Point Titration (IPT) as well as Gran titrations.
  6. Hitachi UV-VIS Model 2100 Spectrophotometer
  7. QuantaChrome Autosorb-1-MP fully automated gas sorption analyzer (BET) for characterization of surface area, pore volume and pore size distribution of microporous and mesoporous solids, providing measurements of surface area ranging from about 0.0005 m2/g to no known upper limits, and measurements of pore size distributions ranging from 3.5 to 4000 angstroms.
  8. RIGAKU SmartLab high-resolution XRD system for powder diffraction analysis (phase analysis), small angle X-ray scattering (SAXS) measurements.

Sample Preparation

  1. Mettler Toledo high precision analytical balances in  laminar flow hoods
  2. Retsch MM400 Mixer Mill for pulverization of samples for microwave digestion, XRD analysis, other analytical or experimental purposes.
  3. Anton Paar MultiWave 3000 Microwave Digester with 8SXF100 high performance rotor/vessels. The digester is equipped with evaporation system and scrubber - used for concentration of samples, evaporation of acids or for silicate removal using HF.
  4. Beckman Coulter Allegra X-22R refrigerated centrifuge with a selection of different rotors
  5. Yamato DX300 convection oven for sample drying etc
  6. Thermo Scientific Thermolyne FB1315M high temperature muffle furnace

Becoming a user

In order to become an instrument user you need to subscribe to our JHA workgroup (ESD Geochemistry Aqueous Geochemistry Lab and Field (Steefel)) and meet the workgroup's training requirements. On-job-training (OJT) is required for all equipment. Training cost vary depending upon instrument and what your needs are. Notice that we will give you training in how to use the instrument, but not in how to do the data analysis nor method development and quality control...

To gain keycard access you also need to take EHS0475 X-ray users, found online here.  

Please fill out this User Agreement Form to become a user. You also need to read the Lab Primer

Fee Basis for ICP-MS

We offer ICP-MS analyses of dissolved and solid phase samples on a per fee basis, although time on the instrument can also be rented by those who prefer to carry out the analyses themselves.  Notice that fees represent what it cost for the service - LDRD/IGPP, G&A etc. are not included (these are usually around 57-58% for most projects).

Prices are effective October 1, 2012.

Self Use

This means that you are renting the instrument for a block of time that you will be charged for on an hourly basis.

Hourly instrument fee:  $76

NOTICE:

  1. You need to sign up for a block of time in advance. You will be charged for that block if you forget to cancel or don’t’ show up on time.  If you are on time, you will only be charged for the actual time you use;
  2.  Initial training required - typically 4 hours at current labor charge;
  3. Training will be given on how to use the instrument, but not on how to do the data analysis nor on method development and quality control;
  4. All sample and standard preparation is the responsibility of the user

Analytical Services

All prices are per sample, based on basic sample preparation consisting of sample dilution and spiking with internal standard where used. For digestion, extraction, filtering, centrifugation or other pre-treatment - additional cost is listed below.
Turn-around time is typically 4 weeks.

  • Semi-quantitative analysis      $21 (72 elements, one analysis, no replicates.)
  • Quantitative analysis              $29 (multiple elements, 5 or more replicates per sample)        
  • Ultra Trace Metal Analysis     $420 (ppt level of trace metals; includes digestion of solid sample, spiking etc)

NOTICE:

  1. We analyze the sample ”as is” - no filtering or pre-treatment unless specified on delivery or requested in an advance.
  2. For spiked or duplicate samples - these count as separate and therefore additional samples
  3. If you request to include analysis of a reference material in addition to your samples - these will count as a separate analysis/sample
  4. When we analyze a sample using a multi-element method, realize that it in order to be efficient—both with regards to analytical time and sample consumption—the method is a compromise between many optimal settings, so certain elements will not always yield the best possible result.
  5. At times the concentration ratio between elements may be so high that two or more dilutions are necessary. For example, a sample in which Na is 1,000 mg/L and Ca is 10 ug/L cannot be analyzed in the same run and require two different dilutions, and thus two separate analyses. Another example is selenium in groundwater samples - often, the Se concentration is very low compared to other elements in the sample, making it unsuitable for accurate determination in the sample in a multi-element method with a standard dilution.
  6. Some elements or group of elements must be analyzed by themselves to get reliable results and will count as separate analyses. Some of these elements are Hg, Au, 99Tc, 210Pb, 226Ra, Br, S+P, rare earth elements REE, platinum group elements PGE. For example, you may have a groundwater sample that you want to analyze for Ca, Fe, Mn + S + Hg. This will then count as three (3) separate analyses.
  7. Ultra Trace Metals Analysis – this means you are measuring certain elements at ppt (or picogram/gram) concentration. The analysis includes:
    • Dissolution of solid sample. If microwave assisted digestion is required, there will be an extra charge per sample (see below)
    • Typically, the dissolved/digested sample will be divided into two sample portions where one is spiked with the most crucial elements. Both sample portions are analyzed, and spike recovery data are reported.  We can also dissolve two samples and spike one. This will still count as one sample for analytical purposes
    • All lab ware has been specially cleaned with UHP (ultra high purity) grade acids to minimize any contamination from the lab ware and checked for cleanliness before use.
    • Preparation work is done in laminar flow hoods to minimize contamination.
  8. A quote can always be obtained before analysis starts to give you an idea what the total cost is likely to be.

Special or Additional Sample Pre-Treatment

  • Microwave assisted digestions (for subsequent ICP-MS analysis). Includes milling of sample if necessary, but not sieving.
    • Cost per sample:  $ 75
  • Other microwave assisted preparation – drying, pre-concentration, HF removal
    • Cost per sample:  $ 75
  • Simple acid digestion, extraction, filtering, centrifugation, pre-concentration, sieving of solid fraction for microwave-assisted digestion.
    • Labor charge per hour:  $ 85

Custom analytical work

This includes:

  • Initial method development for analyses we don’t do on a routine basis.
  • Speciation work (Se, Cr, As, V, Br) using HPLC-ICP-MS
  • Isotope ratio (e.g. 235U/238U, 25Mg/24Mg)
  • Isotope fraction/abundance analysis (% abundance of each isotope)
  • Isotope dilution analysis for the most accurate and precise concentration determination

You will pay the actual cost = labor charges + instrument charges + supplies.


Contact:
Joern T. Larsen, JTLarsen@lbl.gov, 510-486-6165

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