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By: Jack Hall, Quality Assurance Manager Materials and Chemistry Laboratory, Inc. ( McLinc ). Low Level Mercury by Thermo-decomposition of Fish and Soil using Hydra II-C Analyzer. T he ASP 2013 A nnual W orkshop. S tudy G oal :

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low level mercury by thermo decomposition of fish and soil using hydra ii c analyzer

By: Jack Hall, Quality Assurance Manager

Materials and Chemistry Laboratory, Inc. (McLinc)

Low Level Mercury by Thermo-decomposition of Fish and Soil using Hydra II-C Analyzer

The ASP 2013 Annual Workshop

slide2

Study Goal:

Evaluate the Precision and Accuracy of a Thermo-Decomposition Instrument on Fish and Soil.

Materials and Chemistry Laboratory, Inc. (McLinc)

slide3

Teledyne/Leeman Labs Hydra llc

Automated Direct Hg Analyzer

(Total Operation fits on a standard desk top.)

Materials and Chemistry Laboratory, Inc. (McLinc)

slide4

Method based on EPA Method 7473:

  • Mercury in Solids and Solutions by Thermal Decomposition, Amalgamation, and Atomic Absorption Spectrophotometry
  • Determines Total Mercury- OrganicandInorganic (CAS No. 7439-97-6) in the following matrices:
            • Soils
            • Sediments
            • Bottom Deposits
            • Sludge-type Materials
            • Aqueous Wastes
            • Ground Water, and
            • Digested Solutions.

Materials and Chemistry Laboratory, Inc. (McLinc)

slide5

Process Description:

  • Drying & Combusting (decomposition) of a sample at high temperatures with oxygen producing gases.
  • Gases are carried through a heated catalyst that removes:
    • halogens,
    • nitrogen oxides, and
    • sulfur oxides.
    • (continued on next slide)

Materials and Chemistry Laboratory, Inc. (McLinc)

slide6

ProcessDescription (continued):

  • Remaining combustion products (including elemental mercury) are swept through a gold amalgamation tube.
  • Amalgamation tube captures all of the mercury.
  • Amalgamation tube is then heated to release mercury as a gaseous bolus into carrier gas .
    • (continued on next slide)

Materials and Chemistry Laboratory, Inc. (McLinc)

slide7

Process Description (continued):

  • Carrier gas transports to the cold vapor atomic absorption spectrometer (CVAAS).
  • Transient signal measured in series by a high sensitivity cell followed by a low sensitivity cell.
  • Two peaks are integrated and reported against the best calibration of the two cells available.
  • (continued on next slide)

Materials and Chemistry Laboratory, Inc. (McLinc)

slide8

Process Description (continued):

  • Purpose of the two cells is to provide a wider dynamic range of linearity than can be provided by a single optical cell length.

Materials and Chemistry Laboratory, Inc. (McLinc)

slide9

Absorption Cells

(1)

Sample Boat

High Sensitivity

Low Sensitivity

Air

50 to 900C

600C

(4) Drying

Tube

(5) Amalgam

Trap

(6) Spectrometer

(2) Decomposition Furnace

(3)

Catalyst

Furnace

O2 Supply

Principal of Operation

Materials and Chemistry Laboratory, Inc. (McLinc)

slide10

Autosampler Rack

Materials and Chemistry Laboratory, Inc. (McLinc)

slide11

Sample Boat

for

Autosampler

Materials and Chemistry Laboratory, Inc. (McLinc)

slide12

Blank Soil

SRM 2586 Soil

(367±0.038ng/g)

SRM 1947 Lake Michigan

Fish Tissue (254±5ng/g)

Materials and Chemistry Laboratory, Inc. (McLinc)

slide13

Paddlefish Filet caught

near Fort Loudon Dam

in Tennessee

Preparation of Paddlefish

using a Hamilton-Beach Blender

Materials and Chemistry Laboratory, Inc. (McLinc)

slide14

Picture of Paddlefish and Boat Paddle

Materials and Chemistry Laboratory, Inc. (McLinc)

slide15

Paddlefish Sample Preparation

(Sample ID: LD Fish Tissue):

  • Approximately a two pound filet obtained from a paddlefish, caught in the Tennessee River, in Watts Bar Lake, was prepared for mercury analysis.
  • Using a razor blade, the meat of the filet was removed from the skin in small chunks. [Note - no bones were present in the filet.]
  • Next, the meat was placed in a stainless steel blender to thoroughly homogenize and size reduce the chunks.
  • The meat was then transferred to a Teflon® sample bottle to await analysis.

The samples made from standard materials were used as is.

Preparation of Samples for Mercury Analysis

Materials and Chemistry Laboratory, Inc. (McLinc)

slide16

Calibration Standard

Stock Standard #1

UltraScientific, Cat.# ICM-303

Lot# M00317

MCL# CV011

Hg = 100±0.5µg/mL

Matrix: 5% Nitric Acid

Exp. Date: 04-30-2014

Second Source

NIST: SRM2586

Trace Elements in Soil

Hg = 0.367±0.038µg/kg (367ng/g)

LOW Range Rho = 0.9995414

HIGH Range Rho = 0.9997137

LOW Range CCV = 95%R

HIGH Range CCV = 106%R

Stock Standard #1, 0.1ppm Hg

CV011: 0.1mL diluted to 100mL with di-water

Stock Standard #2, 1.0ppm Hg

CV011: 1.0mL diluted to 100mL with di-water

Initial Calibration

Materials and Chemistry Laboratory, Inc. (McLinc)

slide17

Actual Printout of the Low Calibration Curve

Materials and Chemistry Laboratory, Inc. (McLinc)

slide18

Actual Printout of High Calibration Curve

Materials and Chemistry Laboratory, Inc. (McLinc)

slide19

Mean = 9.95 Tng

StdDev = 0.236

MDL = 0.74 Lowest Std/RL, Tng = 5.0

Spiked Soil MDL Study

Materials and Chemistry Laboratory, Inc. (McLinc)

slide20

Mean = 56.71ng/g

StdDev = 4.257

MDL = 13.38 Lowest Std/RL, Tng = 5.0

Paddlefish MDL Study (Fish Tissue)

Materials and Chemistry Laboratory, Inc. (McLinc)

slide21

Mean = 32.24 Tng

StdDev = 2.663

MDL = 8.37 Lowest Std/RL, Tng = 5.0

  • %R - Percent Recovery t=2.896
  • Used 9 runs in MDL calculation: MDL – 1, 2, 4, 6, 7, 8, 9, 10, and 11.

NIST: SRM 1947 Fish Tissue MDL Study

Materials and Chemistry Laboratory, Inc. (McLinc)

slide22

Mean = 43.18 Tng

StdDev = 4.630

MDL = 14.55 Lowest Std/RL, Tng = 5.0

  • %R – Percent Recovery t=2.764
  • Used all 11 runs in MDL calculation.

NIST: SRM 2586 Soil MDL Study

Materials and Chemistry Laboratory, Inc. (McLinc)

mercury in srm 2586 spiked soil vs expected mercury of 367 0 038ng g corrected for weight
Mercury in SRM 2586 Spiked Soil vsExpected Mercury of 367±0.038ng/g(corrected for weight)

Materials and Chemistry Laboratory, Inc. (McLinc)

slide24

Standard SRM 2586 Mercury (Hg) Soil Analysis

Using Different Weights (0.1g, 0.3g, and 0.5g)

Materials and Chemistry Laboratory, Inc. (McLinc)

mercury in srm 1947 fish tissue vs expected mercury of 254 5ng g corrected for weight
Mercury in SRM 1947 Fish Tissue vsExpected Mercury of 254±5ng/g(corrected for weight)

Materials and Chemistry Laboratory, Inc. (McLinc)

ld fish vs srm 2586 spiked soil vs srm 1947 fish tissue
LD Fish vs. SRM 2586 Spiked Soil vs. SRM 1947 Fish Tissue

Materials and Chemistry Laboratory, Inc. (McLinc)

slide27

Conclusions and Recommendations:

  • Simple preparation.
  • Ease of use.
  • Best sample size 0.1 to 0.3g.
  • Great Accuracy (% Recovery) of Soil at low weight.
  • Positive but acceptable Accuracy (Bias) of Fish Tissue.
  • Soil Precision very good with a CV= <0.03
  • Fish Precision also good with a CV = <0.08
  • Thermo Decomposition is Very Suitable for Both Matrices.

Materials and Chemistry Laboratory, Inc. (McLinc)