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


Single mode/

open




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

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


Single mode/

open



Single mode/

open


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

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


Single mode/

open




Multimode/

MP closed


1. 4 min at 30 W,

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


Multimode/

HP closed

Multimode/

HP closed

Multimode/

HP closed


75 sec at 665 W

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


Multimode/

LP closed

Multimode/

LP closed

Multimode/

LP closed

Multimode/

LP closed


1. 6 min at 330 W, cool

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


Multimode/

open


Multimode/

open

(with reflux top)


1. 5 min at 300 W,

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


Single mode/

open




Multimode/

MP closed


1. 4 min at 30 W,

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


Multimode/

LP closed

Multimode/

LP closed


25 min at 70 psi

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


Multimode/

LP closed

Multimode/

LP closed


25 min at 70 psi

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


Multimode/

LP closed

Multimode/

LP closed

Multimode/

HP closed


3 min at 600 W

(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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