Appendix 1. Biological Reference Materials
| Appendix 1.2 Botanical | ||||||
|---|---|---|---|---|---|---|
| Matrix | Analytes | Reagents | Cavity/Vessel | Conditions | Detection | Ref. |
BCR Aquatic plant 60 |
Ca, Cd, Cu, Fe, K, Mg, Mn, Na, Pb, Zn | HNO3, HCl | Multimode/ LP closed |
15 min at 300 W, 5 min at 0 W, 20 min at 510 W |
F-AAS ETV-AAS F-OES |
E72 |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 350 W, 10 min at 140 W |
ETV-AAS | E9 | |
| Fe | A. HNO3 B. 1. HNO3 2. HF |
HP closed Multimode/ HP closed |
Same as A |
ETV-AAS | E6 | |
| 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 | E5 | |
BCR Aquatic moss 61 (contd.) |
Cd | HNO3, HCl | Multimode/ HP closed |
4 min at 360 W, 10 min at 180 W |
ETV-AAS | E4 |
| Cu, Cd, Mn, Pb, Zn | HNO3 | Multimode/ HP closed |
30 sec at 665 W | F-OES F-AAS ICP-OES |
E49 | |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 360 W, 10 min at 180 W |
ICP-OES | E10, E11 | |
BCR Aquatic moss 61 |
Cu, Cd, Mn, Pb, Zn | HNO3 | Multimode/ HP closed |
30 sec at 665 W | F-OES F-AAS ICP-OES |
E49 |
| Fe | A. HNO3 B. 1. HNO3 2. HF |
HP closed Multimode/ HP closed |
Same as A |
ETV-AAS | E6 | |
BCR Aquatic moss 61 (contd.) |
Cd | HNO3, HCl | Multimode/ HP closed |
4 min at 360 W, 10 min at 180 W |
ETV-AAS | E4 |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 350 W, 10 min at 140 W |
ETV-AAS | E9 | |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 360 W, 10 min at 180 W |
ICP-OES | E10, E11 | |
BCR Olive blossom 62 |
Cu, Cd, Mn, Pb, Zn | HNO3 | Multimode/ HP closed |
30 sec at 665 W | F-OES F-AAS ICP-OES |
E49 |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 350 W, 10 min at 140 W |
ETV-AAS | E9 | |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 360 W, 10 min at 180 W |
ICP-OES | E10, E11 | |
| Ca, Cd, Cu, Fe, K, Mg, Mn, Na, Pb, Zn | HNO3, HCl | Multimode/ LP closed |
15 min at 300 W, 5 min at 0 W, 20 min at 510 W |
F-AAS ETV-AAS F-OES |
E72 | |
| Cd, Cu, Mn, 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 | E5 | |
| Pb | HNO3, HCl | Multimode/ flow through |
18 sec at 700 W (0.4 mL coil, 1.5 mL min-1) |
ETV-AAS | E8 | |
| Cu, Mg, Pb | HNO3 | Multimode/ LP closed |
3 min at 650 W | ETV-AAS | E3 | |
BCR Spruce needles 101 |
Cd, Cu, Pb | HNO3, HClO4, H2SO4 | Multimode/ HP closed. |
10 min at 85 bar | DP-ASV | E1 |
| Al, Ca, Mg, Mn, P, Zn | 1. HNO3 2. HNO3 3. H2O2 4. H2O |
Single mode/ open |
1. 5 min at 10 W, 10 min at 30 W, 10 min at 60 W 2. 10 min 60 W 3. 5 min at 60 W 4. 5 min at 50 W |
ICP-OES ICP-MS HPLC-ICP-MS |
E13 | |
BCR Wholemeal flour 189 |
Cd, Cu, Fe, Mn, Zn | A. HNO3, H2O2 B. HNO3, H2O2 C. HNO3, HClO4 |
HP closed Multimode/ HP closed Multimode/ HP closed |
1 min at 250 W, 2 min at 0 W, 2 min at 250 W, 2 min at 400 W, 2 min at 600 W 150 sec at 950 W, 60 sec at 0 W, 90 sec at 300 W, 90 sec at 500 W, 90 sec at 700 W, 90 sec at 850 W |
ETV-AAS | E6 |
BCR Ulva lactuca 279 |
Ca, Cd, Cu, Fe, K, Mg, Mn, Na, Pb, Zn | HNO3 | Multimode/ LP closed |
5 min at 300 W, 5 min at 0 W, 5 min at 300 W, 5 min at 450 W, 5 min at 0 W, 5 min at 450 W |
F-AAS ETV-AAS F-OES |
E72 |
BCR White clover 402 |
Co, Mo | A. 1. HNO3 2. HNO3 3. H2O2 4. H2O B. 1. HNO3, HCl 2. HNO3, HCl 3. H2O2 4. H2O |
open Single mode/ open |
10 min at 30 W, 10 min at 60 W 2. 10 min 60 W 3. 5 min at 60 W 4. 5 min at 50 W 1. 5 min at 40 W, 10 min at 50 W 2. 20 min 54 W 3. 5 min at 40 W 4. 5 min at 50 W |
ICP-OES ICP-MS HPLC-ICP-MS |
E13 |
IAEA Hay powder V10 |
Mo | 1. HNO3 2. Perhydrol |
Multimode/ open then Multimode/ LP closed |
1. 30 min at 180W (open), 10 min at 420W, 10 min at 600W 2. 10 min at 600W |
MS | E73 |
| I | HNO3, N2H4 | Multimode/ HP closed |
35 sec at 675 W | NAA | E17 | |
IAEA Hay powder V10 (contd.) |
Ca, Cd, Cu, Fe, K, Mg, Mn, Na, Pb, Zn | HNO3, HCl | Multimode/ LP closed |
15 min at 300 W, 5 min at 0 W, 20 min at 510 W |
F-AAS ETV-AAS F-OES |
E72 |
| Hg | 1. HNO3 2. H2O2 |
Multimode/ HP closed |
3 min at 450 W | Radiochemical | E30 | |
| Ag, Ba, Bi, Cd, Co, Cr, Cs, Cu, Ga, Hg, Li, Mo, Ni, Pb, Rb, Sn, Sr, Th, U, Zn, Zr | HNO3 | Multimode/ HP closed |
1 min at 300 W (x3-5), 7 min at 300 W, 2 min at 600 W |
ICP/MS | E74 | |
MOE Vegetation V85-1 |
Al, Ba, Ca, Cu, Fe, Mg, Mn, Zn | Aqua regia | Multimode/ stopped flow |
2 min at 720 W or 32 min at 720 W |
ICP-OES | E58 |
MOE Norway maple |
Al, Ba, Ca, Cu, Fe, Mg, Mn, Pb, Zn | A. Aqua regia B. Aqua regia |
stopped flow Multimode/ open |
2 min at 720 W, 2 min at 0 W, 2 min at 720 W, 2 min at 0 W, 2 min at 720 W (with water load) |
ICP-OES | E58 |
MOE White birch |
Al, Ba, Ca, Cd, Cu, Fe, Mg, Mn, Zn | A. Aqua regia B. Aqua regia |
stopped flow Multimode/ open |
2 min at 720 W, 2 min at 0 W, 2 min at 720 W, 2 min at 0 W, 2 min at 720 W (with water load) |
ICP-OES | E58 |
NIES Pepperbush 1 |
Ca, Fe, Mg, Zn | HNO3 | Multimode/ flow through |
100 sec at 525 W (10 mL coil, 6 mL min-1) |
F-AAS | E39 |
| Ca, Cu, Fe, Mg, Mn, Zn | HNO3, HClO4, HCl, HF | Multimode/ MP closed |
14 min intermittent 200 W | F-AAS | E27 | |
NIES Pepperbush 1 (contd.) |
Co | HNO3, HCl | Multimode/ MP closed |
5 min at 600 W (50 mL water load), 5 min at 600 W (no load) |
UV-Vis | E75 |
| Cd, Co, Cu, Ni, Pb | HNO3, HCl, HClO4, HF |
Multimode/ HP closed |
5 min at 200 W (water load), 3.5 min at 200 W (no load) |
ICP-OES ETV-ICP |
E28 | |
| Cd, Cu, Fe, Mn, Zn | A. HNO3, H2O2 B. HNO3, H2O2 C. HNO3, HClO4 |
HP closed Multimode/ HP closed Multimode/ HP closed |
1 min at 250 W, 2 min at 0 W, 2 min at 250 W, 2 min at 400 W, 2 min at 600 W 150 sec at 950 W, 60 sec at 0 W, 90 sec at 300 W, 90 sec at 500 W, 90 sec at 700 W, 90 sec at 850 W |
ETV-AAS | E6 | |
| Fe, Mn, Zn | HNO3 | Multimode/ flow through |
- | F-AAS ICP-OES ICP/MS |
E66 | |
| Cd | 1. HNO3, HClO4, HCl, HF 2. HClO4 |
Multimode/ MP closed |
1. 5 min at 200 W (using water load), 4 min at 200 W (no load) |
F-AAS | E76 | |
NIES Tea leaves 7 |
Ca, Cu, Fe, Mg, Mn, Zn | HNO3, HClO4, HCl, HF | Multimode/ MP closed |
14 min intermittent 200 W | F-AAS | E27 |
| Co | HNO3, HCl | Multimode/ LP closed |
5 min at 600 W (50 mL water load), 5 min at 600 W (no load) |
UV-Vis | E75 | |
| Cd, Co, Cu, Ni, Pb | HNO3, HCl, HClO4, HF |
Multimode/ MP closed |
5 min at 200 W (water load), 3.5 min at 200 W (no load) |
ICP-OES ETV-ICP |
E28 | |
NIES Sargasso 9 |
Ca, Fe, Mg, Zn | HNO3 | Multimode/ flow through |
100 sec at 525 W (10 mL coil, 6 mL min-1) |
F-AAS | E39 |
| Fe, Mn, Zn | HNO3 | Multimode/ flow through |
- | F-AAS ICP-OES ICP/MS |
E66 | |
| As, Cr, V | HNO3, H2O2 | Multimode/ LP closed |
3 min at 300 W | ICP/MS | E77 | |
| Ca, Cu, Fe, Mg, Mn, Zn | HNO3, HClO4, HCl, HF | Multimode/ MP closed |
14 min intermittent 200 W | F-AAS | E27 | |
NIES Rice flour 10 |
Mo | 1. HNO3 2. Perhydrol |
Multimode/ open then Multimode/ LP closed |
1. 30 min at 180W (open), 10 min at 420W, 10 min at 600W 2. 10 min at 600W |
MS | E73 |
| Cd | 1. HNO3, HClO4, HCl, HF 2. HClO4 |
Multimode/ MP closed |
1. 5 min at 200 W (using load), 4 min at 200 W (no load) | F-AAS | E76 | |
NIST Apple leaves 1515 |
Ba, Ce, Co, Cr, Eu, Fe, Hf, K, La, Na, Sb, Sc, Sm, Sr, Tb, Zn | 1. HNO3, HF 2. HClO4 |
Multimode/ LP closed |
1. 20 min at 373 W (9 vessels) 2. 20 min at 545 W (6 vessels) |
NAA | E78 |
NIST Peach leaves 1547 |
Ba, Ce, Co, Cr, Eu, Fe, Hf, K, La, Na, Sb, Sc, Sm, Sr, Tb, Zn | 1. HNO3, HF 2. HClO4 |
Multimode/ LP closed |
1. 20 min at 373 W (9 vessels) 2. 20 min at 545 W (6 vessels) |
NAA | E78 |
NIST Wheat flour 1567 |
Mo | 1. HNO3 2. Perhydrol |
Multimode/ open then Multimode/ LP closed |
1. 30 min at 180 W (open), 10 min at 420 W, 10 min at 600 W 2. 10 min at 600W |
MS | E73 |
| Se | 1. HNO3 2. H2SO4, HClO4 3. H2O |
Single mode/ open |
1. 15 min at 45 W, 10 min at 75 W 2. 10 min at 90 W, 35 min at 120 W 3. 8 min at 120 W |
ETV-AAS | E18 | |
| Cd | HNO3 | Multimode/ LP closed |
2 min on defrost three times | ETV-AAS | E40 | |
| Hg | HNO3 | Multimode/ LP closed |
8 min at 140 W, 8 min at 280 W, 4 min at 420 W |
CV-AAS | E2 | |
| Ba, Ca, K, Mg, Mn, Na, P, S, Zn | 1. HNO3 2. H2O2 |
Multimode/ open |
1. 30 min at 540 W 2. 30 min at 540 W |
ICP-OES | E42 | |
| Residual amino acids | HNO3 | Multimode/ LP closed |
Varied | Fluorimetric | E43 | |
NIST Wheat flour 1567 (contd.) |
Al, Ba, Ca, K, Mg, Mn, Na, P, S, Si, Zn | A. 1. HNO3 2. H2O2 3. H2O2 B. 1. HNO3 2. H2O2, HF 3. H3BO3 |
open Multimode/ open (with reflux top) |
600 W until 1 mL remains 2. 30-40 min at 600 W until 1 mL remains 1. 5 min at 300 W, 20-30 min at 600 W reflux not on 2. 30 min at 180 W reflux on 3. 180 W reflux on |
FI-ICP-OES | E35 |
| Se | HNO3 | Multimode/ LP closed |
(1.5 h at 60°C on hotplate) 4 min at 287 W |
ETV-AAS | E44 | |
| Ca, Cu, Fe, K, Mn, Zn | HNO3 | Multimode/ HP closed |
30 sec at 665 W | F-OES F-AAS ICP-OES |
E49 | |
| As, Ca, Cu, Fe, Mg, Mn, Mo, P, S, Se, U, V, Zn | HNO3, H2O2 | Multimode/ MP closed (Max 350 psi - power cutoff at 150 psi) |
4 min at 296 W, 8 min at 360 W |
F-AAS ICP/MS ICP-OES |
E79 | |
| Cu, Fe, K, Mn, Zn | HNO3 | Multimode/ LP closed |
8 min at 150 W | F-AAS ETV-AAS SIMAAC |
E54 | |
| Ca, Cu, Fe, K, Mg, Mn, P, Zn | HNO3, HCl | Multimode/ LP closed |
5 min at 300 W, 5 min at 0 W, 5 min at 300 W, 5 min at 450 W, 5 min at 0 W, 5 min at 450 W |
ICP-OES | E80 | |
NIST Wheat flour 1567 (contd.) |
Cd, Cu, Fe, Mn | 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 | E5 |
| Ca, Fe, K, Mg, Mn, Na, P, S | 1. HNO3 2. H2O2 3. HCl |
Multimode/ LP closed |
1. 30 min at 540 W, 5 min at 0 W 2. 5 min at 0 W, 15 min at 540 W, 5 min at 0 W 3. 10 min at 180 W |
ICP-OES | E81 | |
NIST Rice flour 1568 |
Ba, Ca, K, Mg, Mn, Na, P, S, Zn | 1. HNO3 2. H2O2 |
Multimode/ open |
1. 30 min at 540 W 2. 30 min at 540 W |
ICP-OES | E42 |
| Residual amino acids | HNO3 | Multimode/ LP closed |
Varied | Fluorimetry | E43 | |
| Al, Ba, Ca, K, Mg, Mn, Na, P, S, Si, Zn | A. 1. HNO3 2. H2O2 3. H2O2 B. 1. HNO3 2. H2O2, HF 3. H3BO3 |
open Multimode/ open (with reflux top) |
600 W until 1 mL remains 2. 30-40 min at 600 W until 1 mL remains 1. 5 min at 300 W, 20-30 min at 600 W reflux not on 2. 30 min at 180 W reflux on 3. 180 W reflux on |
FI-ICP-OES | E35 | |
| B | HNO3, H2O2 | Multimode/ HP closed |
2 min at 100W, 2 min at 0 W, 5 min at 250 W, 3 min at 0 W, 5 min at 500 W, 15 min at 250 W |
UV-Vis Fluorimetry ICP-OES ICP/MS |
E64 | |
| As, Ca, Cu, Fe, Mg, Mn, Mo, P, S, Se, U, V, Zn | HNO3, H2O2 | Multimode/ MP closed (Max 350 psi - power cutoff at 150 psi) |
4 min at 296 W, 8 min at 360 W |
F-AAS ICP/MS ICP-OES |
E79 | |
| Cr, Hg, Se | 1. HNO3 2. H2O2 |
Multimode/ HP closed |
1. 3 min at 450 W | Radiochemical | E30 | |
NIST Spinach 1570 |
I | HNO3, N2H4 | Multimode/ HP closed |
35 sec at 675 W | NAA | E17 |
| Ba, Ca, K, Mg, Mn, Na, P, S, Zn | 1. HNO3 2. H2O2 |
Multimode/ open |
1. 30 min at 540 W 2. 30 min at 540 W |
ICP-OES | E42 | |
NIST Spinach 1570 (contd.) |
Al, Ba, Ca, K, Mg, Mn, Na, P, S, Si, Zn | A. 1. HNO3 2. H2O2 3. H2O2 B. 1. HNO3 2. H2O2, HF 3. H3BO3 |
open Multimode/ open (with reflux top) |
600 W until 1 mL remains 2. 30-40 min at 600 W until 1 mL remains 1. 5 min at 300 W, 20-30 min at 600 W reflux not on 2. 30 min at 180 W reflux on 3. 180 W reflux on |
FI-ICP-OES | E35 |
| Al, Ba, Ca, Cr, Cu, Fe, K, Li, Mg, Mn, Na, P, Si, Sr, Ti, Zn | 1. Aqua regia 2. HBO3 |
Multimode/ MP closed (evacuated slightly at start) |
1. 3 min at 625 W | ICP-OES | E55 | |
NIST Orchard leaves 1571 |
I | HNO3, N2H4 | Multimode/ HP closed |
35 sec at 675 W | NAA | E17 |
| Cd | HNO3 | Multimode/ LP closed |
2 min on defrost three times | ETV-AAS | E40 | |
| As | HNO3, HClO4, H2SO4 | Multimode/ HP closed. |
10 min at 85 bar | DP-ASV | E1 | |
| Al, Ba, Ca, K, Mg, Mn, Na, P, S, Si, Zn | A. 1. HNO3 2. H2O2 3. H2O2 B. 1. HNO3 2. H2O2, HF 3. H3BO3 |
open Multimode/ open (with reflux top) |
600 W until 1 mL remains 2. 30-40 min at 600 W until 1 mL remains 1. 5 min at 300 W, 20-30 min at 600 W reflux not on 2. 30 min at 180 W reflux on 3. 180 W reflux on |
FI-ICP-OES | E35 | |
| As, Co, Cr, Cu, Ni, Pb, Se, Zn | HNO3, HClO4 | Multimode/ open |
600 W until first signs of HClO4 fumes | F-AAS NAA |
E46, E47, E48 | |
NIST Orchard leaves 1571 (contd.) |
Cd | 1. HNO3, HClO4, HCl, HF 2. HClO4 |
Multimode/ MP closed |
1. 5 min at 200 W (using water load), 4 min at 200 W (no load) |
F-AAS | E76 |
| Al, Ba, Ca, Cr, Co, Cu, Fe, K, Mg, Mn, Na, P , S, Zn | HNO3 | Multimode/ LP closed |
10 min at 70 psi, 15 min at 450 W |
NAA ICP-OES |
E22 | |
| Po | HNO3 | Multimode/ MP closed |
60 min at 60 W, cool 60 min at 60 W |
a-spectrometry | E82 | |
| Cd, Co, Fe, Ni, Pb | HNO3, HF | Multimode/ LP closed |
1 min at 240 W, cool (x15) | ETV-AAS X-ray Fluorescence |
E83 | |
| Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, P, Zn | 1. Aqua regia 2. HBO3 |
Multimode/ MP closed (evacuated slightly at start) |
3 min at 625 W | ICP-OES | E55 | |
| Se | HNO3, HClO4 | Not reported | - | Fluorimetry | E65 | |
| Cu, Pb, Zn | HNO3, HClO4 | Multimode/ open |
3 min at 600 W | ETV-AAS | E84 | |
| Al, Ba, Ca, Cu, Fe, Mg, Pb, Zn | A. Aqua regia B. Aqua regia |
stopped flow Multimode/ open |
2 min at 720 W, 2 min at 0 W, 2 min at 720 W, 2 min at 0 W, 2 min at 720 W (with water load) |
ICP-OES | E58 | |
| Al | HNO3 | Multimode/ HP closed |
1 min at 150 W, 30 min at 0 W, 1 min at 450 W |
ICP-OES | E20 | |
NIST Citrus leaves 1572 |
Al, Ag, As, Ba, Ca, Cl, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, N, Na, Ni, P, Pb, Rb, S, Sb, Si, Sr, Ti, Zn | HNO3, HClO4 | Multimode/ MP closed |
15 min at 0 W, 10 min at 150 W, 10 min at 450 W, 15 min at 0 W |
ICP-OES | E31 |
| I | HNO3, N2H4 | Multimode/ HP closed |
35 sec at 675 W | NAA | E17 | |
| Cd | HNO3 | Multimode/ LP closed |
2 min on defrost three times | ETV-AAS | E40 | |
| Ba, Ca, K, Mg, Mn, Na, P, S, Zn | 1. HNO3 2. H2O2 |
Multimode/ open |
1. 30 min at 540 W 2. 30 min at 540 W |
ICP-OES | E42 | |
NIST Citrus leaves 1572 (contd.) |
Al, Ba, Ca, K, Mg, Mn, Na, P, S, Si, Zn | A. 1. HNO3 2. H2O2 3. H2O2 B. 1. HNO3 2. H2O2, HF 3. H3BO3 |
open Multimode/ open (with reflux top) |
600 W until 1 mL remains 2. 30-40 min at 600 W until 1 mL remains 1. 5 min at 300 W, 20-30 min at 600 W reflux not on 2. 30 min at 180 W reflux on 3. 180 W reflux on |
FI-ICP-OES | E35 |
| - | HNO3 | Multimode/ LP closed |
10 min at 360 W, 5 min at 480 W | - | E85 | |
| Cd | 1. HNO3, HClO4, HCl, HF 2. HClO4 |
Multimode/ MP closed |
1. 5 min at 200 W (using water load), 4 min at 200 W (no load) |
F-AAS | E76 | |
| Hg | HNO3 | Multimode/ LP closed |
800 W until 75°C, 3 min at 75°C |
CV-FANES | E86 | |
| Hg | HNO3 | Multimode/ HP closed |
90 sec at 600 W (estimated power) |
CV-AAS | E87 | |
| Al | HNO3 | Multimode/ MP closed |
4 min at 200 W, cool, 4 min at 350 W, cool, 8 min at 250 W, cool, 10 min at 400 W (x4) |
ETV-AAS | E88 | |
| Sr | HNO3 | Multimode/ open |
Heat until dryness. | ID (stable isotope dilution activation analysis) | E89 | |
| As, Ca, Cu, Fe, Mg, Mn, Mo, P, S, Se, U, V, Zn | HNO3, H2O2 | Multimode/ MP closed (Max 350 psi - power cutoff at 150 psi) |
4 min at 296 W, 8 min at 360 W |
F-AAS ICP/MS ICP-OES |
E79 | |
NIST Citrus leaves 1572 (contd.) |
Ca, Cu, Fe, K, Mg, Mn, P, Zn | HNO3, HCl | Multimode/ LP closed |
5 min at 300 W, 5 min at 0 W, 5 min at 300 W, 5 min at 450 W, 5 min at 0 W, 5 min at 450 W |
ICP-OES | E80 |
| As, Cr, Hg, Sb | 1. HNO3 2. H2O2 |
Multimode/ HP closed |
3 min at 450 W | Radiochemical | E30 | |
| Ba, Ca, Cu, Mg, Mn, Zn | 1. HNO3, HF 2. HBO3 |
Multimode/ LP closed |
2 min at 240 W, 2 min 360 W, 16 min at 160°C (600W) |
ICP-OES | E90 | |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 350 W, 10 min at 140 W |
ETV-AAS | E9 | |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 360 W, 10 min at 180 W |
ICP-OES | E10, E11 | |
| Al, Ca, Fe, K, Mg, Mn, Na, P, S | 1. HNO3 2. H2O2 3. HCl |
Multimode/ LP closed |
1. 30 min at 540 W, 5 min at 0 W 2. 5 min at 0 W, 15 min at 540 W, 5 min at 0 W 3. 10 min at 180 W |
ICP-OES | E81 | |
| P | 1. HNO3, HClO4 2. HClO4 |
Multimode/ open (with scrubber) |
1. 15 min at 750 W | ICP-OES | E91 | |
| Al | HNO3, H2SO4 | Multimode/ MP closed |
5 min at 1170 W | IC | E92 | |
| As | HNO3, H2O2 | Multimode/ HP closed |
- | ICP/MS | E93 | |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 460 W, 10 min at 180 W (10 mL water load) |
ICP-OES | E94 | |
NIST Citrus leaves 1572 (contd.) |
Cu, Fe, Mn, 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 | E5 |
| Ca, Fe, K, Mg, Mn, Zn | - | Multimode/ open |
30 min at 650 W | F-AAS | E95 | |
| Ca, Cu, Fe, Mg, Mn, K, Na, Zn | 1. HNO3 2. HNO3 3. H2O2 |
Single mode/ open |
1. 10 min at 60 W, 5 min at 80 W 2. 5 min at 70 W 3. 3 min at 60 W |
F-AAS | E67 | |
| Al | HNO3 | Multimode/ HP closed |
1 min at 150 W, 30 min at 0 W, 1 min at 450 W |
ICP-OES | E20 | |
| Al, As, Ba, Cr, Cu, Fe, K, Mg, Mn, Ni, P, Pb, Rb, Sr, Zn | 1. HNO3 2. HF 3. H2O2 |
Multimode/ HP closed |
1. 5 min at 300 W, 2 min at 600 W, 2 min at 0 W, 3 min at 300 W 2. 5 min at 300 W, 2 min at 600 W, 2 min at 0 W 3. 5 min at 300 W, 2 min at 600 W, 2 min at 0 W, 3 min at 300 W |
DCP-OES F-AAS |
E96 | |
NIST Tomato leaves 1573 |
Cu, Mn | HNO3, H2O2 | Multimode/ flow through |
2 min at 650 W (digestate recirculated through oven) | F-AAS | E97 |
| Ba, Ca, K, Mg, Mn, Na, P, S, Zn | 1. HNO3 2. H2O2 |
Multimode/ open |
1. 30 min at 540 W 2. 30 min at 540 W |
ICP-OES | E42 | |
| Al, Ba, Ca, K, Mg, Mn, Na, P, S, Si, Zn | A. 1. HNO3 2. H2O2 3. H2O2 B. 1. HNO3 2. H2O2, HF 3. H3BO3 |
open Multimode/ open (with reflux top) |
600 W until 1 mL remains 2. 30-40 min at 600 W until 1 mL remains 1. 5 min at 300 W, 20-30 min at 600 W reflux not on 2. 30 min at 180 W reflux on 3. 180 W reflux on |
FI-ICP-OES | E35 | |
| As, Cr, Cu, Fe, Mn, Pb, Rb, Sr, Th, U, Zn | 1. HNO3 2. HF |
Multimode/ MP closed |
1. Leave overnight, 3 min at 130 W, 6 min at 195 W, 6 min at 260 W, 6 min at 325 W, cool, vent 2. 6 min at 325 W |
ICP/MS | E98 | |
| Cd | 1. HNO3, HClO4, HCl, HF 2. HClO4 |
Multimode/ MP closed |
1. 5 min at 200 W (using water load), 4 min at 200 W (no load) |
F-AAS | E76 | |
NIST Tomato leaves 1573 (contd.) |
Ca, Cu, Fe, K, Mn, P, Pb, Zn | HNO3 | Multimode/ HP closed |
30 sec at 665 W | F-OES F-AAS ICP-OES |
E49 |
| Sr | HNO3 | Multimode/ open |
Heat until dryness. | ID (stable isotope dilution activation analysis) | E89 | |
| Al, Ba, Ca, Cd, Cr, Fe, K, Mg, Mn, Na, P | 1. Aqua regia 2. HBO3 |
Multimode/ MP closed (evacuated slightly at start) |
3 min at 625 W | ICP-OES | E55 | |
| Cd, Co, Fe, Ni, Pb | HNO3, HF | Multimode/ LP closed |
1 min at 240 W, cool (x15) |
ETV-AAS X-ray Fluorescence |
E83 | |
| Cr, Hg, Se | 1. HNO3 2. H2O2 |
Multimode/ HP closed |
3 min at 450 W | Radiochemical | E30 | |
| Fe | A. HNO3 B. 1. HNO3 2. HF |
HP closed Multimode/ HP closed |
Same as A |
ETV-AAS | E6 | |
| Ca, Fe, K, Mg, Mn, Zn | - | Multimode/ open |
30 min at 650 W | F-AAS | E95 | |
| B | HNO3, H2O2 | Multimode/ HP closed |
2 min at 100W, 2 min at 0 W, 5 min at 250 W, 3 min at 0 W, 5 min at 500 W, 15 min at 250 W |
UV-Vis Fluorimetry ICP-OES ICP/MS |
E64 | |
NIST Tomato leaves 1573 (contd.) |
Mn | HNO3 | Multimode/ flow through |
2 sec at 650 W (0.5 mL coil, 15.4 mL min-1) |
F-AAS | E99 |
| Al, As, Be, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Sb, Se, V, Zn | Aqua regia | Multimode/ LP closed |
10 min at 300 W, 5 min at 600 W, 10 min at 480 W | ICP-OES ETV-AAS |
E56 | |
| Ca, Fe, K, Mg, Mn, Na, P, S | 1. HNO3 2. H2O2 3. HCl |
Multimode/ LP closed |
1. 30 min at 540 W, 5 min at 0 W 2. 5 min at 0 W, 15 min at 540 W, 5 min at 0 W 3. 10 min at 180 W |
ICP-OES | E81 | |
NIST Pine needles 1575 |
Pb | HNO3, HCl | Multimode/ flow through |
18 sec at 700 W (0.4 mL coil, 1.5 mL min-1) |
ETV-AAS | E8 |
| Ba, Ca, K, Mg, Mn, Na, P, S, Zn | 1. HNO3 2. H2O2 |
Multimode/ open |
1. 30 min at 540 W 2. 30 min at 540 W |
ICP-OES | E42 | |
NIST Pine needles 1575 (contd.) |
Al, Ba, Ca, K, Mg, Mn, Na, P, S, Si, Zn | A. 1. HNO3 2. H2O2 3. H2O2 B. 1. HNO3 2. H2O2, HF 3. H3BO3 |
open Multimode/ open (with reflux top) |
600 W until 1 mL remains 2. 30-40 min at 600 W until 1 mL remains 1. 5 min at 300 W, 20-30 min at 600 W reflux not on 2. 30 min at 180 W reflux on 3. 180 W reflux on |
FI-ICP-OES | E35 |
| Al, As, Cr, Cu, Fe, Hg, Mn, Pb, Rb, Sr, Th, U | 1. HNO3 2. HF |
Multimode/ MP closed |
1. Leave overnight, 3 min at 130 W, 6 min at 195 W, 6 min at 260 W, 6 min at 325 W, cool, vent 2. 6 min at 325 W |
ICP/MS | E98 | |
| Ca, Cu, Fe, K, Mn, P, Pb | HNO3 | Multimode/ HP closed |
30 sec at 665 W | F-OES F-AAS ICP-OES |
E49 | |
| Hg | HNO3 | Multimode/ LP closed |
800 W until 75°C, 3 min at 75°C |
CV-FANES | E86 | |
NIST Pine needles 1575 (contd.) |
As, Ca, Cu, Fe, Mg, Mn, Mo, P, S, Se, U, V, Zn | HNO3, H2O2 | Multimode/ MP closed (Max 350 psi - power cutoff at 150 psi) |
4 min at 296 W, 8 min at 360 W |
F-AAS ICP/MS ICP-OES |
E79 |
| Al, Ba, Ca, Cr, Fe, K, Mg, Mn, Na, P, Zn | 1. Aqua regia 2. HBO3 |
Multimode/ MP closed (evacuated slightly at start) |
1. 3 min at 625 W | ICP-OES | E55 | |
| Al, As, Be, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Sb, Se, V, Zn | Aqua regia | Multimode/ LP closed |
10 min at 300 W, 5 min at 600 W, 10 min at 480 W | ICP-OES ETV-AAS |
E56 | |
| Cd, Co, Fe, Ni, Pb | HNO3, HF | Multimode/ LP closed |
1 min at 240 W, cool (x15) |
ETV-AAS XRF |
E83 | |
NIST Pine needles 1575 (contd.) |
Ca, Fe, K, Mg, Mn, Na, P, S | 1. HNO3 2. H2O2 3. HCl |
Multimode/ LP closed |
1. 30 min at 540 W, 5 min at 0 W 2. 5 min at 0 W, 15 min at 540 W, 5 min at 0 W 3. 10 min at 180 W |
ICP-OES | E81 |
| Ca, K, Mg, P | 1. HNO3, HClO4 2. HClO4 |
Multimode/ open (with scrubber) |
15 min at 750 W | ICP-OES | E91 | |
| Pb | HNO3 | Multimode/ LP closed |
3 min at 650 W | ETV-AAS | E3 | |
| Al | HNO3 | Multimode/ LP closed |
40 sec at 700 W, 10 min at 0 W (vent), 60 sec at 700 W, 10 min at 0 W (vent), 90 sec at 700 W, 5 min at 70 W |
ETV-AAS | E63 | |
| Cu | 1. HNO3 2. H2O2 |
Multimode/ LP closed |
9.5 min at 540 W | F-AAS | E100 | |
NIST Pine needles 1575 (contd.) |
Cu, Fe, 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 | E5 |
| B | HNO3, H2O2 | Multimode/ HP closed |
2 min at 100W, 2 min at 0 W, 5 min at 250 W, 3 min at 0 W, 5 min at 500 W, 15 min at 250 W |
UV-Vis Fluorimetry ICP-OES ICP/MS |
E64 | |
| Ca, Fe | HNO3, HCl, HF | Multimode/ MP closed |
15 min at 540 W | DCP-OES | E101 | |
| Al, As, Ba, Cr, Cu, Fe, K, Mg, Mn, Ni, P, Pb, Rb, Sr, Zn | 1. HNO3 2. HF 3. H2O2 |
Multimode/ HP closed |
1. 5 min at 300 W, 2 min at 600 W, 2 min at 0 W, 3 min at 300 W 2. 5 min at 300 W, 2 min at 600 W, 2 min at 0 W 3. 5 min at 300 W, 2 min at 600 W, 2 min at 0 W, 3 min at 300 W |
DCP-OES F-AAS |
E96 | |
NIST Corn stalks 8412 |
Al, Ba, Ca, K, Mg, Mn, Na, P, S, Si, Zn | A. 1. HNO3 2. H2O2 3. H2O2 B. 1. HNO3 2. H2O2, HF 3. H3BO3 |
open Multimode/ open (with reflux top) |
600 W until 1 mL remains 2. 30-40 min at 600 W until 1 mL remains 1. 5 min at 300 W, 20-30 min at 600 W reflux off 2. 30 min at 180 W reflux on 3. 180 W reflux on |
FI-ICP-OES | E35 |
NIST Corn kernel 8413 |
Al, Ba, Ca, K, Mg, Mn, Na, P, S, Si, Zn | A. 1. HNO3 2. H2O2 3. H2O2 B. 1. HNO3 2. H2O2, HF 3. H3BO3 |
open Multimode/ open (with reflux top) |
600 W until 1 mL remains 2. 30-40 min at 600 W until 1 mL remains 1. 5 min at 300 W, 20-30 min at 600 W reflux not on 2. 30 min at 180 W reflux on 3. 180 W reflux on |
FI-ICP-OES | E35 |
| Pb | HNO3, V2O5 | Multimode/ HP closed |
90 sec at 460 W | ETV-AAS | E104 | |
| Hg | HNO3 | Multimode/ HP closed |
90 sec at 600 W | CV-AAS | E105 | |
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