(Modified from Tessier et al., 1979)
Note: read through entire procedure before starting
Note: use wet sample weights; determine moistures at 105°C and correct analytical data
Weigh 1.000g samples into 50ml centrifuge tubes
Add 8ml 1M MgCl2 solution
Agitate frequently at room temperature for 1 hr
Centrifuge, decant, add 4ml aqua regia, and dilute analytical fraction to 1L with Nanopure water
Wash residue with deionized water (Not Nanopure)
Use residue from previous leach
Add 8ml 1M sodium acetate solution adjusted to pH 5.0 with acetic acid Agitate periodically at room temperature for 5 hours
Centrifuge, decant, add 4ml aqua regia, and dilute analytical fraction to 1L with Nanopure water
Wash residue with deionized water (Not Nanopure)
Use residue from previous leach
Add 20ml 0.04M NH20H*HCI in 25% (v/v) acetic acid
Agitate periodically in boiling water bath for 5 hours
Centrifuge, decant, add 4ml aqua regia, and dilute analytical fraction to 1L with Nanopure water
Wash residue with deionized water (Not Nanopure)
Use residue from previous leach
dd 3ml 0.02M HN03 and 5ml of 30% H202 which has been adjusted to pH 2 with HN03
Agitate periodically at 85°C for 2 hours
Add 3ml of H202 (pH 2)
Agitate periodically at 85°C for 3 hours
Cool to room temperature
Add 5 ml of 3.2 M ammonium acetate in 20% v/v HN03
Agitate periodically at room temperature for 30 minutes
Centrifuge, decant, add 4ml aqua regia, and dilute analytical fraction to 1L with Nanopure water
Wash residue with deionized water (Not Nanopure)
Use residue from previous leach
Add 10ml HF and 16ml aqua regia
Heat in hot water bath for 2 hours
Dilute to 1L with Nanopure water
Digest 400mg sample with 8ml aqua regia
Dilute to 500ml with Nanopure water
- or -
Digest 400mg sample with 2ml HF and 8ml aqua regia Dilute to 500ml with Nanopure water
(August 20, 2003)