Appendix 1. Biological Reference Materials
| Appendix 1.3 Marine | ||||||
|---|---|---|---|---|---|---|
| Matrix | Analytes | Reagents | Cavity/Vessel | Conditions | Detection | Ref. |
BCR Mussel tissue 278 |
As | HNO3, H2O2 | Multimode/ LP closed |
1 min at 555 W, 4 min at 300 W |
ETV-AAS | E102 |
| Cu, Pb | HNO3, HClO4, H2SO4 | Multimode/ HP closed |
10 min at 85 bar | DP-ASV | E1 | |
| Cd | HNO3, V2O5 | Multimode/ HP closed |
90 sec at 600 W | ETV-AAS | E103 | |
| Pb | HNO3, V2O5 | Multimode/ HP closed |
90 sec at 460 W | ETV-AAS | E104 | |
| Hg | HNO3 | Multimode/ HP closed |
90 sec at 460 W | CV-AAS | E105 | |
BCR Plankton 414 |
Cd, Cr, Cu, Hg, Mn, Ni, Pb, V, Zn | 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 |
BCR Cod muscle 422 |
Cu | HNO3, HClO4, H2SO4 | Multimode/ HP closed |
10 min at 85 bar | DP-ASV | E1 |
BCR Cod muscle 422 (contd.) |
As, Cu, Fe, Hg, Mn, Zn | A. 1. HNO3 2. HNO3 3. H2O2 4. H2O B. 1. HNO3, HCl 2. HNO3, HCl 3. H2O2 4. H2O C. 1. HNO3, H2SO4 2. HNO3 3. H2O2 4. H2O2 5. H2O |
open Single mode/ 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 1. 5 min at 20 W, 10 min at 40 W, 10 min at 100 W 2. 10 min at 100 W 3. 5 min at 100 W 4. 5 min at 100 W 5. 5 min at 80 W |
ICP-OES ICP-MS HPLC-ICP-MS |
E13 |
IAEA Copepod MAA-1 |
Cr, Hg, Se | 1. HNO3 2. H2O2 |
Multimode/ HP closed |
1. 3 min at 450 W | Radiochemical | E30 |
IAEA Fish flesh MAA-2 |
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 |
| As | HNO3, HClO4, H2SO4 |
Multimode/ HP closed. |
10 min at 85 bar | DP-ASV | E1 | |
| Cr, Hg, Se | 1. HNO3 2. H2O2 |
Multimode/ HP closed |
1. 3 min at 450 W | Radiochemical | E30 | |
IAEA Mussel tissue MAM-2 |
Cr, Hg, Se | 1. HNO3 2. H2O2 |
Multimode/ HP closed |
1. 3 min at 450 W | Radiochemical | E30 |
NIES Chlorella 3 |
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 | |
| 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 | |
NIES Chlorella 3 (contd.) |
I | 1. HNO3 2. N2H4 |
Multimode/ MP closed |
35 sec at 675 W | NAA | E17 |
NIES Mussel 6 |
Ca, Fe, Mg, Zn | HNO3 | Multimode/ flow through |
100 sec at 525 W (10 mL coil, 6 mL min-1) |
F-AAS | E39 |
| Ca, Cd, Cu, Fe, K, Mg, Mn, Na, P, Sr, Zn, Residual carbon | A. 1. HNO3, H2SO4 2. H2O2(x16) 3. HNO3 or HNO3, HCl or NH3 (aq) 4. NH4EDTA B. HNO3 |
open Multimode/ MP closed |
4 min at 120 W 2. 1 min at 120 W(x16) 3. 4 min at 30 W 2 min at 20 psi, 5 min at 40 psi, 2 min at 60 psi, 2 min at 80 psi, 2 min at 100 psi, 2 min at 120 psi, 2 min at 140 psi, 15 min at 160 psi |
ICP-OES | E24 | |
| 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 | |
| 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 | |
| Se | 1. HNO3, H2SO4 2. H2O2 3. H2O2 |
Multimode/ LP closed |
1. 6 min at 330 W, cool 2. 4 min at 450 W, cool 3. 4 min at 600 W |
DPP | E106 | |
NIES Mussel 6 (contd.) |
Se | A. 1. HNO3 2. H2O2 3. H2O2 B. 1. HNO3, H2SO4 2. H2O2 3. H2O2 C. 1. HNO3, H3PO4 2. H2O2 3. H2O2 D. 1. HNO3, K2S2O8 2. H2O2 3. H2O2 |
LP closed Multimode/ LP closed Multimode/ LP closed Multimode/ LP closed |
2. 4 min at 450 W, cool 3. 4 min at 600 W Same as A Same as A Same as A |
HG-AAS | E107 |
| Fe, Mn, Zn | HNO3 | Multimode/ flow through |
- | F-AAS ICP-OES ICP/MS |
E66 | |
| Ca, Cu, Fe, Mg, Mn, Zn | HNO3, HClO4, HCl, HF | Multimode/ MP closed |
14 min intermittent 200 W | F-AAS | E27 | |
| 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 | |
NIST Albacore tuna 50 |
Hg | HNO3 | Multimode/ HP closed |
70 sec at 600 W | CV-AAS | E16 |
NIST Oyster tissue 1566 |
Zn, Cd | HNO3 | Multimode/ open |
8 min at 200 W | FI-F-AAS | E38 |
| I | 1. HNO3 2. N2H4 |
Multimode/ HP closed |
1. 35 sec at 675 W | NAA | E17 | |
| Hg | HNO3 | Multimode/ LP closed |
8 min at 140 W, 8 min at 280 W, 4 min at 420 W |
CV-AAS | E2 | |
| Hg | HNO3 | Multimode/ LP closed |
8 min at 140 W, 8 min at 280 W, 4 min at 420 W |
CV-AFS | E7 | |
| 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 | |
| As | HNO3, H2O2 | Multimode/ LP closed | 1 min at 555 W, 4 min at 300 W | ETV-AAS | ||
NIST Oyster tissue 1566 (contd.) |
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 | |
| As, Ca, Cd, Cu, Fe, K, Mg, Mn, Na, Pb, Zn | HNO3 | Multimode/ HP closed |
30 sec at 665 W | F-OES F-AAS ICP-OES |
E49 | |
| Al, As, Ba, Ca, Cd, Ce, Cr, Cs, Cu, Fe, La, Li, Mg, Mn, Mo, Ni, Rb, Sb, Se, Sr, Tl, V, Y, Zn | HNO3 | Multimode/ MP closed |
75 sec at 350 W | ICP/MS | E21 | |
| 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 | |
| Al, As, Ba, Ca, Cd, Cu, Fe, K, 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 | |
| Hg, Se | 1. HNO3 2. H2O2 |
Multimode/ HP closed |
1. 3 min at 450 W | Radiochemical | E30 | |
| Cu, Fe, Zn | 1. HNO3 2. HClO4, HF |
Multimode/ LP closed |
Variable | SPC-IC | E57 | |
| Residual carbon | HNO3 | Multimode/ HP closed |
5 min at 500 W (200 bar) |
Total carbon analyzer Carbon dioxide coulometer |
E59 | |
NIST Oyster tissue 1566 (contd.) |
Ca, Cd, Cu, Fe, K, Mg, Mn, Na, P, Sr, Zn, Residual carbon | A. 1. HNO3, H2SO4 2. H2O2(x16) 3. HNO3 or HNO3, HCl or NH3 (aq) 4. NH4EDTA B. HNO3 |
open Multimode/ MP closed |
4 min at 120 W 2. 1 min at 120 W(x16) 3. 4 min at 30 W 2 min at 20 psi, 5 min at 40 psi, 2 min at 60 psi, 2 min at 80 psi, 2 min at 100 psi, 2 min at 120 psi, 2 min at 140 psi, 15 min at 160 psi |
ICP-OES | E24 |
| As, arsenocholine, arsenobetaine, tetramethylarsonium iodide | HNO3 | Multimode/ HP closed |
90 sec at 500 W | ETV-AAS | E108 | |
| Cd, Cr, Cu, Mn, Mo, Pb | HNO3 | Multimode/ LP closed |
3 min at 650 W | ETV-AAS | E3 | |
| Cd, Cu, Mn, Pb, Zn | HNO3, H2SO4 | Multimode/ open |
1000 W until nitric acid boils off | F-AAS | E109 | |
NRCC Dogfish liver DOLT-1 |
Cu, Fe, Zn | HNO3 | Multimode/ HP closed |
3 min at 418 W | F-AAS | E110 |
| Residual carbon | HNO3 | Multimode/ HP closed |
5 min at 500 W (200 bar) |
Total carbon analyzer Carbon dioxide coulometer |
E59 | |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 350 W, 10 min at 140 W |
ETV-AAS | E9 | |
| As, Se | HNO3, H2O2 | Multimode/ LP closed |
3 min at 300 W | ICP/MS | E77 | |
| Cd | HNO3, HCl | Multimode/ HP closed |
4 min at 360 W, 10 min at 180 W |
ETV-AAS | E4 | |
| Cu, Fe, Zn | HNO3 | Multimode/ HP closed |
- | ICP-OES F-AAS |
E111 | |
| Cu, Fe, Zn | HNO3 | Multimode/ HP closed |
3 min at 418 W | F-AAS | E112 | |
NRCC Dogfish liver DOLT-1 (contd.) |
Hg, Se | HNO3 | Multimode/ LP closed |
8 min at 75 W, 8 min at 225 W, 4 min at 375 W |
CV-AAS HG-AAS |
E113 |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 360 W, 10 min at 180 W |
ICP-OES | E10, E11 | |
NRCC Dogfish muscle DORM-1 |
Hg, Se | HNO3 | Multimode/ LP closed |
8 min at 75 W, 8 min at 225 W, 4 min at 375 W |
CV-AAS HG-AAS |
E113 |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 350 W, 10 min at 140 W |
ETV-AAS | E9 | |
| As, dimethylarsenic acid, arsenite, monomethylarsonic acid, arsenate, methanearsonate | HNO3 | Multimode/ LP closed |
- | HPLC-ICP/MS | E114 | |
| As, Cr | HNO3, H2O2 | Multimode/ LP closed |
3 min at 300 W | ICP/MS | E77 | |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 460 W, 10 min at 180 W (10 mL water load) |
ICP-OES | E94 | |
| Cd | HNO3, HCl | Multimode/ HP closed |
4 min at 360 W, 10 min at 180 W |
ETV-AAS | E4 | |
| Residual carbon | HNO3 | Multimode/ HP closed |
5 min at 500 W (200 bar) |
Total carbon analyzer Carbon dioxide coulometer |
E59 | |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 360 W, 10 min at 180 W |
ICP-OES | E10, E11 | |
NRCC Non-defatted lobster hepatopancreas LUTS-1 |
Residual carbon | HNO3 | Multimode/ HP closed |
5 min at 500 W (200 bar) |
Total carbon analyzer Carbon dioxide coulometer |
E59 |
| Cd, Co, Cu, Hg, Mn, Ni, Pb, Sr, Zn | 1. HNO3 2. H2O2 |
Multimode/ LP closed |
1. 10 min at 3.5 atm 2. 5 min at 4 atm |
ICP/MS | E115 | |
| Cd | HNO3 | Multimode/ LP closed |
2 min at 600 W, 10 min at 90 W |
ASV | E116 | |
NRCC Cod liver tissue NOAA-K |
Ag, As, Cd, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Sn, Zn | A. HNO3, HClO4 B. HNO3 |
LP closed Multimode/ LP closed |
Same as A |
ICP/MS | E117 |
NRCC Shellfish tissue NOAA-L |
Ag, As, Cd, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Sn, Zn | A. HNO3, HClO4 B. HNO3 |
LP closed Multimode/ LP closed |
Same as A |
ICP/MS | E117 |
NRCC Lobster hepatopancreas TORT-1 |
As, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Se, Zn | HNO3, HClO4 | Multimode/ LP closed |
20 min at 60-65 psi | ETV-AAS F-AAS |
E118 |
| As, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Se, Sr, V, Zn | A. HNO3, H2O2 B. HNO3, H2O2 C. HNO3, H2O2 |
LP closed Multimode/ LP closed Multimode/ HP closed |
(Pressure release) 1 min at 600 W 1 min at 600 W |
ETV-AAS F-AAS |
E119 | |
| Cd, Cr, Pb | HNO3 | Multimode/ LP closed |
15 min at 180 W, 10 min at 0 W, 15 min at 180 W |
F-AAS | E120 | |
| As, Ni, Co | HNO3, HClO4, H2SO4 | Multimode/ HP closed. |
10 min at 85 bar | DP-ASV | E1 | |
| Residual carbon | HNO3 | Multimode/ HP closed |
5 min at 500 W (200 bar) |
Total carbon analyzer Carbon dioxide coulometer |
E59 | |
| As, Cd, Co, Cr, Cu, Mn, Ni, Pb, Sn, V, Zn | HNO3 | Multimode/ MP closed |
5 min at 60W, 5 min at 90 W, 15 min at 150 W |
ETV-AAS F-AAS |
E121 | |
| As | HNO3, H2O2 | Multimode/ HP closed |
- | ICP/MS | E93 | |
NRCC Lobster hepatopancreas TORT-1 (contd.) |
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 |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 350 W, 10 min at 140 W |
ETV-AAS | E9 | |
| As, Cr, Se, V | HNO3, H2O2 | Multimode/ LP closed |
3 min at 300 W | ICP/MS | E77 | |
| Ni | HNO3, HCl | Multimode/ HP closed |
4 min at 460 W, 10 min at 180 W (10 mL water load) |
ICP-OES | E94 | |
| 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 360 W, 10 min at 180 W |
ICP-OES | E10, E11 | |
| Ca, Cu, Fe, Zn | HNO3, HCl, HF | Multimode/ MP closed |
15 min at 540 W | DCP-OES | E101 | |
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