| Appendix 2.3 Soils and sediments | ||||||
|---|---|---|---|---|---|---|
| Matrix | Analytes | Reagents | Cavity/Vessel | MW conditions | Detection | Ref. |
| BCR
Calcareous loam 141 |
Cd, Cr, Cu, Fe, Mn, Pb, Zn | HCl, HNO3 | Multimode/
LP closed |
1 min at 180 W, 4 min at 480 W,
60 min at 600 W |
F-AAS
ETV-AAS |
F35 |
| Cd, Cu, Pb | 1. HNO3, H2O, H2O2
2. Aqua regia, HF (optional) |
Multimode/
open |
1. 15 min at 70 W,
15 min at 150 W, 15 min at 180 W, 1 min at 250 W, 1 min at 600 W 2. 15 min at 70 W, 1 min at 600 W |
ETV-AAS | F36 | |
| BCR
Soil - light sandy 142 |
Cd, Cr, Cu, Fe, Mn, Pb, Zn | HCl, HNO3 | Multimode/
LP closed |
1 min at 180 W,
4 min at 480 W, 60 min at 600 W |
F-AAS
ETV-AAS |
F35 |
| BCR
Estuarine sediment 277 |
As, Cd, Cr, Cu, Hg, Ni, Pb, Zn | A.
1. HCl, HNO3 2. HCl, HNO3 3. H2O2 4. H2O B. HCl, HNO3, HF |
Single mode/
open
Multimode/ LP closed |
1. 5 min at 40 W, 10 min at 50 W
2. 10 min at 54 W 3. 5 min at 40 W 4. 5 min at 50 W 10 min at 120 W, 20 min at 240 W, 20 min at 300 W |
ICP-OES
ICP-MS CV-AAS HPLC-ICP-MS |
F37 |
| CANMET
Regosolic C horizon soil SO-1 |
As | 1. HNO3
2. HNO3, HClO4, H2SO4 |
Multimode/
LP closed |
1. 2.5 min at 639 W, cool, vent
2. 2.5 min at 639 W, 2 min 0 W (x3) |
F-AAS | F38 |
| Pb | HNO3, HF | Multimode/
LP closed |
7 min at 400 W | DP-ASV | F39 | |
| CANMET
Podzolic B horizon soil SO-2 |
As | 1. HNO3
2. HNO3, HClO4, H2SO4 |
Multimode/
LP closed |
1. 2.5 min at 639 W, cool, vent
2. 2.5 min at 639 W, 2 min 0 W (x3) |
F-AAS | F38 |
| Pb | HNO3, HF | Multimode/
LP closed |
7 min at 400 W | DP-ASV | F39 | |
| CANMET
Calcareous C horizon soil SO-3 |
As | 1. HNO3
2. HNO3, HClO4, H2SO4 |
Multimode/
LP closed |
1. 2.5 min at 639 W, cool, vent
2. 2.5 min at 639 W, 2 min 0 W (x3) |
F-AAS | F38 |
| CANMET
Calcareous C horizon soil SO-3 (contd.) |
Pb | HNO3, HF | Multimode/
LP closed |
7 min at 400 W | DP-ASV | F39 |
| CANMET
Black Chernozemic A horizon soil SO-4 |
As | 1. HNO3
2. HNO3, HClO4, H2SO4 |
Multimode/
LP closed |
1. 2.5 min at 639 W, cool, vent
2. 2.5 min at 639 W, 2 min 0 W (x3) |
F-AAS | F38 |
| Pb | HNO3, HF | Multimode/
LP closed |
7 min at 400 W | DP-ASV | F39 | |
| IAEA
Lake sediment SL-1 |
Al, Ba, Ca, Cr, Cu, Fe, K, Li, Mg, Mn, Na, P, Pb, Si, Sr, Ti, V, Zn | Aqua regia, HF | Multimode/
open |
3 min at 625 W | ICP-OES | F21 |
| Cd, Cr, Cu, Fe, Mn, Pb, Zn | HCl, HNO3 | Multimode/
LP closed |
1 min at 180 W, 4 min at 480 W,
60 min at 600 W |
F-AAS
ETV-AAS |
F35 | |
| IAEA
Soil 5 |
Hg | HCl, HNO3, H2O | Multimode/
LP closed |
1 min at 180 W, 4 min at 480 W,
10 min at 600 W |
CV-AAS
NAA |
F40 |
| IAEA
Soil 7 |
Cd, Cr, Cu, Fe, Mn, Pb, Zn | HCl, HNO3 | Multimode/
LP closed |
1 min at 180 W, 4 min at 480 W,
60 min at 600 W |
F-AAS
ETV-AAS |
F35 |
| IGGE
Stream sediment GSD-2 |
Al, Be, Cr, K, La, Li, Nb, Si, Sn, Ti, Y, Zr | 1. HNO3, HCl, HF
2. H3BO3 |
Multimode/
LP closed |
1. 2.5 min at 650 W
2. 10 min at 650 W |
ICP-OES | F2 |
| IGGE
Stream sediment GSD-3 |
Al, Cr, K, La, Li, Si, Ti, V, Zr | 1. HNO3, HCl, HF
2. H3BO3 |
Multimode/
LP closed |
1. 2.5 min at 650 W
2. 10 min at 650 W |
ICP-OES | F2 |
| IGGE
Stream sediment GSD-8 |
Al, K, Li, Nb, Si, Sn, Ti, Y, Zr | 1. HNO3, HCl, HF
2. H3BO3 |
Multimode/
LP closed |
1. 2.5 min at 650 W
2. 10 min at 650 W |
ICP-OES | F2 |
| NIES
Pond sediment 2 |
Hg | HNO3 | Multimode/
HP closed |
70 sec at 600 W | CV-AAS | F41 |
| NIST
River sediment 1645 |
Ca, Cr, Fe, Mn, Pb, Zn | Exchangeable:
MgCl2 Carbonate Bound: Sodium Acetate Fe-Mn Oxide: Hydroxylamine hydrochloride Organic: H2O2, HNO3 Residual: HNO3, HCl, HF |
Multimode/
open Multimode/ open Multimode/ open Multimode/ open Multimode/ open |
4 min at ? W
5 min at ? W 4 min at ? W (x3) 4 min at ? W 5 min at ? W |
F-AAS | F42 |
| Al, As, Ba, Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P, Pb, Si, Sr, Ti, Zn | Aqua regia, HF | Multimode/
open |
3 min at 625 W | ICP-OES | F21 | |
| Al, K, Li, Si | 1. HNO3, HCl, HF
2. H3BO3 |
Multimode/
LP closed |
1. 2.5 min at 650 W
2. 10 min at 650 W |
ICP-OES | F2 | |
| Th, U | 1. HCl, HNO3, HF
2. Aqua regia |
Multimode/
HP closed |
1. 4-8 min at 600 W,
fume off acid (x3) 2. If residue 3 min at 600 W |
a spectrometry | F7 | |
| Hg | HNO3 | Multimode/
LP closed |
Heat to 75°C (800 W),
2 min at 75°C |
CV-FANES | F43 | |
| As, Cd, Cu, Mg, Mn, Ni, Pb, Zn | HNO3, H2O | Multimode/
LP closed |
Heat to 100 psi,
55 min at 100 psi |
- | F44 | |
| Al, Ba, Ca, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Sc, Si, Ti, V, Zn, Zr | 1. HF, Aqua regia
2. H3BO3 |
Multimode/
LP closed |
1. 8 min at 300 W,
4 min at 600 W, 7 min at 480 W 2. 6 min at 600 W |
ICP-OES | F20 | |
| Al, As, Ba, Ca, Cd, Cr, Cu, Co, Fe, K, Mg, Mn, Na, Ni, Pb, Sb, Sc, Se, Si, Sn, Ti, Tl, V, Zn, Zr | 1. HF, Aqua regia
2. H3BO3 |
Multimode/
LP closed |
1. 8 min at 300 W,
11 min at 600 W 2. 6 min at 300 W |
ICP-OES
F-AAS ETV-AAS |
F6 | |
| NIST Estuarine sediment
1646 |
Al, As, Ba, Ca, Cd, Cr, Cu, Co, Fe, K, Mg, Mn, Na, Ni, Pb, Sb, Sc, Se, Si, Sn, Ti, Tl, V, Zn, Zr | 1. HF, Aqua regia
2. H3BO3 |
Multimode/
LP closed |
1. 8 min at 300 W,
11 min at 600 W 2. 6 min at 300 W |
ICP-OES
F-AAS ETV-AAS |
F6 |
| Ca, Cr, Fe, Mn, Pb, Zn | Exchangeable:
MgCl2 Carbonate Bound: Sodium Acetate Fe-Mn Oxide: Hydroxylamine hydrochloride Organic: H2O2, HNO3 Residual: HNO3, HCl, HF |
Multimode/
open Multimode/ open Multimode/ open Multimode/ open Multimode/ open |
4 min at ? W
5 min at ? W 4 min at ? W (x3) 4 min at ? W 5 min at ? W |
F-AAS | F42 | |
| Al, As, B, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, Pb, Ti, V, Zn | HNO3 | Multimode/
LP closed |
10 min at 400 W
50 min at 330 W |
ICP-OES | F45 | |
| Al, Ba, Ca, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Sc, Si, Ti, V, Zn, Zr | 1. HF, Aqua regia
2. H3BO3 |
Multimode/
LP closed |
1. 8 min at 300 W,
4 min at 600 W, 7 min at 480 W 2. 6 min at 600 W |
ICP-OES | F20 | |
| NIST
Buffalo river sediment 2704 |
As, Cr, Cu, Mn, Ni, Pb, Se, Zn | HNO3, H2O | Multimode/
LP closed |
12 min to 100 psi (651 W),
30 min at 100 psi (651 W, 181°C) |
F-AAS
ETV-AAS |
F46 |
| Ag, Al, B, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, Sr, V, Zn | HNO3 | Multimode/
LP closed |
5.5 min to 175°C (574 W),
4.5 min at 175-180°C (574 W) |
ICP-OES | F47, F48 | |
| Ag, As, Ba, Cd, Cu, Cr, Hg, Ni, Pb, Se, Tl, Zn | A.
HNO3 B. HNO3, HF |
Multimode/
LP closed Multimode/ LP closed |
2:20 min at 600 W,
9:25 min at 480 W Same as A |
ETV-AAS
CV-AAS |
F49 | |
| Ag, As, Ba, Cd, Cu, Cr, Hg, Ni, Pb, Sb, Se, Tl, Zn | Extraction:
HNO3 Total: HNO3, HF |
Multimode/
LP closed Multimode/ LP closed |
2:20 min at 604 W,
9:25 min at 570 W Same as extraction |
F50 | ||
| NIST
Buffalo river sediment 2704 (contd.) |
Ba, Cd, Cr, Co, Cu, Pb, Ni, Sr, V, Zn | HNO3 | Multimode/
LP closed |
5.5 min to 175°C (574 W),
4.5 min at 175-180°C (574 W) |
F51 | |
| Co, Cr, Cu, Ni, Pb, Zn | A.
1. HF, HNO3, HCl 2. H3BO3 B. HNO3 C. Same as A D. 1. HF, HNO3 2. H3BO3 E. HNO3, HCl F. Same as A G. Same as E H. HF, HNO3, HCl I. HNO3, H2O2 J. HNO3, H2O2, HF K. 1. HNO3, H2O2, HF 2. H3BO3 L. Acetic acid M. Same as E N. Same as H |
Multimode/
LP closed (all same) |
8 min at 630 W,
15 min at 315 W Same as A 10 min at 630 W, 20 min at 473 W, 5 min at 158 W Same as C Same as C 10 min at 630 W, 20 min at 410 W, 5 min at 189 W 10 min at 630 W, 20 min at 441 W, 5 min at 158 W 15 min at 630 W Same as G Same as G Same as G Same as G 7 min at 441 W, 5 min at 630 W Same as M |
F-AAS
ETV-AAS |
F52,
F53 |
|
| NIST
Buffalo river sediment 2704 (contd.) |
Al, As, Ba, Be, Ca, Co, Cr, Cu, Fe, Hg, Mg, Mn, Ni, P, Pb, S, Se, Tl, U, V, Zn | HNO3 | Multimode/
LP closed |
Heat to 175°C within 5.5 min,
4.5 min at 175-180°C |
ICP-MS
ETV-AAS |
F54 |
| Cd, Cr, Cu, Ni, Pb, Zn | A.
HNO3 B. HNO3, HF |
Multimode/
LP closed Multimode/ LP closed |
Heat to 175°C within 5.5 min,
4.5 min at 175-180°C Heat to 175°C within 5.5 min, 9.5 min at 175-180°C |
F-AAS
ETV-AAS ICP-MS |
F55 | |
| NIST
Montana soil highly elevated traces 2710 |
Cd, Cr, Cu, Ni, Pb, Zn | A.
HNO3 B. HNO3, HF |
Multimode/
LP closed Multimode/ LP closed |
Heat to 175°C within 5.5 min, 4.5 min at 175-180°C
Heat to 175°C within 5.5 min, 9.5 min at 175-180°C |
F-AAS
ETV-AAS ICP-MS |
F55 |
| NIST
Montana soil moderately elevated traces 2711 |
Cd, Cr, Cu, Ni, Pb, Zn | A.
HNO3 B. HNO3, HF |
Multimode/
LP closed Multimode/ LP closed |
Heat to 175°C within 5.5 min, 4.5 min at 175-180°C
Heat to 175°C within 5.5 min, 9.5 min at 175-180°C |
F-AAS
ETV-AAS ICP-MS |
F55 |
| NIST
Peruvian soil 4355 |
As, Cr, Cu, Mn, Ni, Pb, Se, Zn | HNO3, H2O | Multimode/
LP closed |
12 min to 100 psi (651 W),
30 min at 100 psi (651 W/181°C) |
F-AAS
ETV-AAS |
F46 |
| Ag, Al, B, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, Sr, V, Zn | HNO3 | Multimode/
LP closed |
5.5 min to 175°C (574 W),
4.5 min at 175-180°C (574 W) |
ICP-OES | F47,F48 | |
| NRCC
Marine sediment BCSS-1 |
Al, Ba, Be, Ca, Cd, Cr, Cu, Fe, Hg, Mg, Mn, Na, Ni, P, Pb, Sr, Ti, V, Zn | HNO3, HCl | Multimode/
LP closed |
1-20 min at 720 W | ICP-OES
ETV-AAS |
F56 |
| Al, As, Ba, Be, Ca, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, S, Sb, Ti, V, Zn | A.
Aqua regia B. 1. Aqua regia, HF 2. H3BO3 |
Multimode/
LP closed Multimode/ LP closed |
2 min at 600 W,
5 min at 360 W, 15 min at 180 W 1. 1 min at 600 W, 5 min at 360 W, 15 min at 180 W 2. 15 min at 330 W |
ICP-OES
NAA |
F23 | |
| NRCC
Marine sediment MESS-1 |
Al, Cr, K, Li, Si, Ti, Zr | 1. HNO3, HCl, HF
2. H3BO3 |
Multimode/
LP closed |
1. 2.5 min at 650 W
2. 10 min at 650 W |
ICP-OES | F2 |
| Si, Al, Zn, Cr | HCl, HNO3, HF | Multimode/
LP closed |
50 - 60 sec at 700 W | F-AAS | F27 | |
| Al, Ba, Be, Ca, Cd, Cr, Cu, Fe, Hg, Mg, Mn, Na, Ni, P, Pb, Sr, Ti, V, Zn | HNO3, HCl | Multimode/
LP closed |
1-20 min at 720 W | ICP-OES
ETV-AAS |
F56 | |
| Al, As, Ba, Be, Ca, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, S, Sb, Ti, V, Zn | A.
Aqua regia B. 1. Aqua regia, HF 2. H3BO3 |
Multimode/
LP closed Multimode/ LP closed |
2 min at 600 W,
5 min at 360 W, 15 min at 180 W 1. 1 min at 600 W, 5 min at 360 W, 15 min at 180 W 2. 15 min at 330 W |
ICP-OES
NAA |
F23 | |
| As, Cd, Co, Cr, Cu, Mn, Ni, Pb, Sn, V, Zn | HNO3, HF | Multimode/
MP closed |
25 min at 210 W | ETV-AAS
F-AAS |
F57 | |
| As, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Se, Zn | A.
HNO3, HF, HClO4 B. Same as A |
Multimode/
LP closed Multimode/ LP closed |
100% power to 60-65 psi,
20 min at 65 psi Heat as in A, vent, repeat A |
F-AAS
ETV-AAS ICP-OES |
F58 | |
| NRCC
Marine Sediment PACS-1 |
As, Cr, Cu, Mn, Ni, Pb, Se, Zn | HNO3, H2O | Multimode/
LP closed |
12 min to 100 psi (651 W),
30 min at 100 psi (651 W/181°C) |
F-AAS
ETV-AAS |
F46 |
| Al, As, Ba, Be, Ca, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, S, Sb, Ti, V, Zn | A.
Aqua regia B. 1. Aqua regia, HF 2. H3BO3 |
Multimode/
LP closed Multimode/ LP closed |
2 min at 600 W,
5 min at 360 W, 15 min at 180 W 1. 1 min at 600 W, 5 min at 360 W, 15 min at 180 W 2. 15 min at 330 W |
ICP-OES
NAA |
F23 | |
| NRCC
Soil SO-2 |
Cu, Zn | HNO3, HF | Multimode/
LP closed |
15 min at 105 W, vent,
7 min at 350 W |
F-AAS | F59 |
| NRCC
Soil SO-3 |
Cu, Zn | HNO3, HF | Multimode/
LP closed |
15 min at 105 W, vent,
7 min at 350 W |
F-AAS | F59 |
| NRCC
Soil SO-4 |
Cu, Zn | HNO3, HF | Multimode/
LP closed |
15 min at 105 W, vent,
7 min at 350 W |
F-AAS | F59 |
| RMA
Standard soil |
Ag, As, Ba, Cd, Cu, Cr, Hg, Ni, Pb, Se, Tl, Zn | A.
HNO3 B. HNO3, HF |
Multimode/
LP closed Multimode/ LP closed |
2:20 min at 600 W,
9:25 min at 480 W Same as A |
ETV-AAS
CV-AAS |
F49 |
| Ag, As, Ba, Cd, Cu, Cr, Hg, Ni, Pb, Sb, Se, Tl, Zn | Extraction:
HNO3 Total: HNO3, HF |
Multimode/
LP closed Multimode/ LP closed |
2:20 min at 604 W,
9:25 min at 570 W Same as extraction |
F50 | ||
| USGS
Soil GXR-2 |
Al, K, Li, Si, Ti, Zr | 1. HNO3, HCl, HF
2. H3BO3 |
Multimode/
LP closed |
1. 2.5 min at 650 W
2. 10 min at 650 W |
ICP-OES | F2 |
| Nb, Mo, Ta, W | 1. HNO3
2. HF, H2O |
Multimode/
MP closed |
1. 30 min at 200 W
2. 1 min at 1000 W, 30 min at 450 W |
ID-ICP-MS | F9 | |
| USGS
Fe-Mn-W rich hot spring deposit GXR-3 |
Al, K, Li, Mg, Si, Ti | 1. HNO3, HCl, HF
2. H3BO3 |
Multimode/
LP closed |
1. 2.5 min at 650 W
2. 10 min at 650 W |
ICP-OES | F2 |
| USGS
Soil GXR-5 |
Al, Cr, K, Li, Si, Ti, Zr | 1. HNO3, HCl, HF
2. H3BO3 |
Multimode/
LP closed |
1. 2.5 min at 650 W
2. 10 min at 650 W |
ICP-OES | F2 |
| Nb, Mo, Ta, W | 1. HNO3
2. HF, H2O |
Multimode/
MP closed |
1. 30 min at 200 W
2. 1 min at 1000 W, 30 min at 450 W |
ID-ICP-MS | F9 | |
| USGS
Marine sediment MAG-1 |
Nb, Mo, Ta, W | 1. HNO3
2. HF, H2O |
Multimode/
MP closed |
1. 30 min at 200 W
2. 1 min at 1000 W, 30 min at 450 W |
ID-ICP-MS | F9 |
| Al, K, Li, Si, Ti, Y, Zr | 1. HNO3, HCl, HF
2. H3BO3 |
Multimode/
LP closed |
1. 2.5 min at 650 W
2. 10 min at 650 W |
ICP-OES | F2 | |