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Woods Hole Field Center

Geochemical Sediment Analysis Procedures

U.S. Geological Survey Open-File Report 02-371

by S.A. Jablonski, E.L. Mecray, J.M. Munson, and D.S. Blackwood

Well Gamma Procedure 
  Analytical Laboratories
  Total and Organic Carbon Analysis - CHN
  Inorganic Carbon Analysis - Coulometer
  Biogenic Silica Analysis
  Radiochemistry (Gamma Analysis)
  Acid Washing Procedure
  Drying Procedures
  Sediment Grinding Procedures
  Geochemistry - Core Sectioning Procedure
  Weighing Samples
  Job Hazard Analysis
  Material Safety Data Sheets  (non-USGS link )



The Woods Hole Field Center (WHFC) has the capability to measure organic, inorganic, and total carbon contact using Coulometer and CHN Analyzers. Total and organic carbon percentages are determined using the Perkin Elmer 2400 Series II CHN Analyzer (Figure 1). From these analyses, one can determine the percent inorganic carbon of a sediment sample by subtracting the percent organic carbon from the percent total carbon:
%total carbon = %inorganic carbon + %organic carbon. Another instrument available for the determination of inorganic carbon content in sediment, is the UIC Coulometrics, Inc. Carbon Dioxide Coulometer with an acidification unit
(Figure 2).

The organic carbon fraction in sediments is important because it serves as a binding site for contaminant metals. The abundance of organic carbon controls many diagenic processes. Normalizing contaminant data by the % organic carbon allows for the distinction of specific anthropogenic sources.

CHN Analyzer; link to larger image
Figure 1. Perkin Elmer Series II CHN Analyzer.

Coulometer with acidification unit; link to larger image
Figure 2. Coulometer with Acidification Unit

CHN Analyzer procedures - The CHN Analyzer uses a combustion method to convert the sample elements to simple gases (CO2, H2O, and N2). The dried and ground sediment sample is first oxidized using classical reagents like Silver Vanadate, Silver Tungstate, and EA-1000, which is mixture of chrome and nickel oxides. Products produced in the combustion zone include CO2, H2O, and N2. Elements such as halogens and sulfur are removed by scrubbing agents in the combustion zone. The resulting gases are homogenized and controlled to exact conditions of pressure, temperature, and volume. The homogenized gases are allowed to de-pressurize through a column where they are separated in a stepwise steady-state manner and quantified as a function of their thermal conductivities (Perkin Elmer Instruction Manual).

In order to measure %organic carbon in sediment samples, one must first acidify the samples to remove all inorganic matter. The inorganic material is removed by adding sulfurous acid to the sediment so the inorganics will turn to gas and leave the sample. Using this method, only the organic material is analyzed by the CHN Analyzer (Verardo, David J. et. al).

Coulometer procedures - The Coulometer provides an accurate and absolute determination of the concentration of carbon dioxide (CO2) evolved from an acidification process. The coulometer cell is filled with a cathode and an anode solution (proprietary through UIC) with a colorimetric indicator. A platinum cathode and a silver anode are positioned in the cell and the assembly is positioned between a light source and a photodetector in the coulometer. When a gas stream passes through the solution, CO2 is quantitatively absorbed, reacting with the elements in the cathode/anode solutions to form a titratable acid. This acid causes the color indicator to fade. Photodetection monitors the change in the solution's color as percent transmittance (%T). As the %T increases, the titration current is automatically activated to stoichiometrically generate a base at a rate proportional to the %T. When the solution returns to its original color (original %T), the current stops (UIC Coulometrics Instruction Manual).

Equipment used for these procedures includes the instruments described above (Perkin Elmer 2400 Series II CHN Analyzer and a UIC Coulometrics Coulometer with an Acidification Unit), as well as a ball-mill grinder used to grind the dried sediment sample to a fine powder, ovens used to insure the sample is dry, desiccators used to cool and store samples in a moisture-free environment, and the chemicals involved in the analysis process.


This laboratory is equipped to handle wet sediment samples (cores and grabs) as they are returned from field collection. Samples are collected from marine and coastal areas and returned to the laboratory for analysis. Cores are sectioned and sub-sampled using titanium tools to minimize contamination (Figure 3). Samples from cores and grabs are freeze-dried (Figure 4) and sent to contract laboratories for various analyses including toxicity tests, mercury concentrations, foraminifera identification, pollen counting, nitrogen isotope analysis, and organic and inorganic contaminant concentrations.

Core sectioning procedures - A fully illustrated tutorial on the methods used at the Woods Hole Field Center is presented in this publication.

Freeze Drying procedures - A fully illustrated tutorial on the methods used at the Woods Hole Field Center is presented in this publication.

Freeze drying is a process whereby water is removed from frozen materials by converting the frozen water directly into its vapor without the intermediate formation of liquid water. The basis for this sublimation process involves: the use of a vacuum pump to enhance the removal of water vapor from the surface of the sample; the transfer and deposition of water vapor onto the condenser; the removal of heat, due to ice formation, from the condenser by means of a refrigeration system. In essence, the freeze dry process is a balance between the heat absorbed by the sample to vaporize the water and the heat removed from the condenser to convert the water vapor into ice (LABCONCO Instruction Manual).
The vacuum environment is important as it speeds the sublimation process by removing atmospheric pressure which would act to contain the molecules in liquid form.

Cutting a core; link to larger image Figure 3. Sampling a core using a hydraulic extruder.



Freeze Dryer unit; link to larger image

Figure 4. Freeze Dryer unit

Equipment used for the procedures in this laboratory includes the instrumentation mentioned above (hydraulic core extruder and freeze dryer), as well as acid-washing baths to clean the titanium spatulas, and a sample splitter to get a non-biased sub-sample.


This laboratory is equipped to determine gamma decay emissions from dried sediment samples. This method allows for the determination of the sample's age and the sedimentation rates in sediment cores. Two types of gamma detectors are used: well-type (Figure 5) and planar-type (Figure 6). These high purity germanium (HPGe) detectors are in constant use and are located in a shared laboratory on the Woods Hole Oceanographic campus.

Radioisotopes, such as Pb-210 and Cs-137, can be measured by gamma emission and used in conjunction with a numerical model to estimate sedimentation rates. These measurements are important in modeling chronological changes such as heavy metal pollution. The WHFC conducts studies in the New York Bight (NYB) and in Long Island Sound (LIS) because they are in close proximity to high-density population centers and sewage dumping. Anthropogenic sources have added metals, carbon, bacteria, and organic contaminants to the sea floor. Although these pollutants have been dispersed over time, they are still present in the sedimentary record and can be measured. Cs-137 is a fallout isotope produced from bomb tests in the 1950's and 1960's and since it is not a naturally occurring isotope, it is known that the onset date for this isotope is 1954 and this information can be used to date the sediment cores collected from those areas (Santschi et al, 1999).

Inside the well-type detector; link to larger image Figure 5. Well-type Gamma Detector.




Planar-type detector; link to larger image
Figure 6. Planar-type Gamma Detector

Well and Planar-type detector procedures - A fully illustrated tutorial on the methods used at the Woods Hole Field Center is provided in this publication. These detectors produce output pulses directly proportional to the energy of the gamma ray. The HPGe detectors are semiconductor diodes and require liquid nitrogen to cool the system reducing the leakage current and therefore reducing the noise and increasing the resolution.

Freeze Dryer procedures - A fully illustrated tutorial on the methods used at the Woods Hole Field Center is provided in this publication.

Instrumentation for these procedures requires both a well-type and a planar-type HPGe detector and a freeze dryer unit.

Biogenic Silica:

The WHFC has the capability to digest sediment samples to be further analyzed by Inductively Coupled Plasma - Emission Spectrometry (ICP-ES) for biogenic silica. Biogenic silica fluxes indicate ecosystem productivity over time. The WHFC does not, at this time, have the instrumentation to analyze the biogenic silica extracts, so contract laboratories are used.

Biogenic silica digestion procedures - A fully illustrated tutorial on the methods used at the Woods Hole Field Center is provided in this publication. The method used is adapted from Mortlock, R.A. et. al (1989).

Equipment for this procedure includes a heated shaker bath (Figure 7) to resuspend the sediment and a centrifuge
(Figure 8) to help remove the supernatent, as well as ovens to dry sediment samples, a mortar and pestle to grind the sediment samples, a balance to weigh samples, a vortexer to swirl the samples, a sonicator to break up sample particles, and the chemicals used in the preparation of the sediment samples.

Heated Shaker Bath; link to larger image
Figure 7. Heated Shaker Bath.

Inside the centrifuge; link to larger image
Figure 8. Centrifuge.

This report is preliminary and has not been reviewed for conformity with U.S. Geological Survey editorial standards (or with the North American Stratigraphic Code). Any use of trade, product, or firm names is for descriptive purposes only and does not imply endorsement by the U.S. government. [an error occurred while processing this directive]