'"
" 0
Table 14.1.
Conditions used for hydride generation
Method
Batch/S-C Purging gas
Reagents
Conditions
Re-arrangement,
DL
References
~
(")
HG-CT-QF-AAS
Helium
6 N HCI (O.5mll. di- and monomethyl standards
Degassing (3 min)
Rearrangement not reported Standards
Andreae et al. 1981,
' "'
~.
100 ml min- 1
(0.05-20ng of Sb) made up with water (lOOml),
Reaction and purge (6 min)
only 52.5 and 42% pure DL
= 30-60 pg
Andreae and
OQ
4% w/w NaBH, (1 mil stabilised with NaOH
Froelich 1984
en
HG-GC-AAS
Helium
pH 1.5-6 range, in water sol. (60 ml), ±KI, tris-(hydroVolatile hydrides were passed through
Rearrangements occurred under all
Dodd et al. 1992
~
.."
xymethyl)-amino-methane, HCI, tri- and dimethyllead acetate trap and a CO/isopropanol
conditions
0
antimony standards, 4% KBfI (6 mil
trap before reaching the column
;a
(l)
' "'
HG-GC-MS
S-C
Helium
i)
1 M HCI, ii) 4 M acetic acid, trim ethyl antimony
Stibines swept through gas-liquid sepaNo rearrangement, when acetic acid, NaBH, Dodd et al. 1996
standards, sample, 2%
mlv NaBH, in 0.1% m/v NaOH
rator, through CO/acetone trap to GC
and distilled water rinsed apparatus, occurs
::0
when only rinsed with distilled water,
p
DL
= 15 ng ofSb
';b'
::s
a) HG-GC -AAS
a) S-C
a) Helium
(CH,),SbCI, (100-200 ng), sample (0.1-3 mil. pH 0.51
a) HG and trapping on column
= 3 min a) No rearrangement at pH 6.10-6.76, reKoch et al. 1998
5b) HG-CTb) B
b) Helium
to 6.76 using various acids and buffers, 2% w/v NaBH,
b) Reaction mixture purged
= 6 min
arrangement at pH 0.51-3.30 (max
= 24%),
'"
ICP-MS
80ml min- 1
b) de-ionised water (10 mil, (CHl)lSbCI, (1 ng),
CO/acetone trap used
sample matrix affects rearrangement,
p
1 M HCI (re-distilled), 6% w/v NaBH, (0.8 ml)
DL
= 4 ng; b) pH similar results to a)
:-tI
max. rearr. 68%, DL
= 0.01 ng
~
HG-CT-AAS
Helium
In millipore-Q water (53 mll.acetic acid (3 mil,
Purged and collected on (old trap
Jenkins et al.
~
' "'
40 ml min- 1
trimethylantimony standard (4.9 ~I),
NaBH, (10 mg)
1998b,(
~
HG-CT-ICP-MS
Helium
Sample (1 g), bidistilled H,O (5 mil. HCI, pH 2
Degassing(l min), purging (10 min)
Rearrangement not reported
Krupp et al. 1996
0
400 ml min- 1
5% NaSH, (1.5 mil
'"
or
HG,
6% m/m NaBH, (purged with H, for 30 min) (0.5 ml)
Conducted in a sealed vial (15 ml)
No rearrangement reported, only
Feldmann et al.
::r
a) GC-ICP-MS
(CHl)lSbCI, (30 ng as Sb), deionised water(l mil, pH 7
injected onto column using a
trimethylantimony detected
1998
t-'
b) GC-MS-MS
Helium
gas-tight syringe
~
a) Sample (4 mil. 0.05 M citrate buffer pH 6, 2% NaSH,
en
a) HG-GC-AAS
a) S-C
Helium
b) Degassing (1 min), purge and
a) and b) No rearrangement seen
Andrewes et al.
3
b) HG-GC-ICP-MS b) B
70 ml min- 1
b) water (10 ml), 6% NaSH, (0.8 ml)
trapping (6 min) column in liq. N,
1998
s:
HG-CT-GCHelium
Sample (condensed water) (10 mil. 5% NaBH, (1 ml),
Degassing (10 min)
No rearrangement reported
Feldmann et al.
~
-1
ICP-MS
500 ml min, degassing pH 2 acidified with 1 M HCI (1.5 ml)
1994
?>
100 ml min purging
s::
0
' "'
::l.
'"
" 0
Table 14.1.
Conditions used for hydride generation
Method
Batch/S-C Purging gas
Reagents
Conditions
Re-arrangement,
DL
References
~
(")
HG-CT-QF-AAS
Helium
6 N HCI (O.5mll. di- and monomethyl standards
Degassing (3 min)
Rearrangement not reported Standards
Andreae et al. 1981,
' "'
~.
100 ml min- 1
(0.05-20ng of Sb) made up with water (lOOml),
Reaction and purge (6 min)
only 52.5 and 42% pure DL
= 30-60 pg
Andreae and
OQ
4% w/w NaBH, (1 mil stabilised with NaOH
Froelich 1984
en
HG-GC-AAS
Helium
pH 1.5-6 range, in water sol. (60 ml), ±KI, tris-(hydroVolatile hydrides were passed through
Rearrangements occurred under all
Dodd et al. 1992
~
.."
xymethyl)-amino-methane, HCI, tri- and dimethyllead acetate trap and a CO/isopropanol
conditions
0
antimony standards, 4% KBfI (6 mil
trap before reaching the column
;a
(l)
' "'
HG-GC-MS
S-C
Helium
i)
1 M HCI, ii) 4 M acetic acid, trim ethyl antimony
Stibines swept through gas-liquid sepaNo rearrangement, when acetic acid, NaBH, Dodd et al. 1996
standards, sample, 2%
mlv NaBH, in 0.1% m/v NaOH
rator, through CO/acetone trap to GC
and distilled water rinsed apparatus, occurs
::0
when only rinsed with distilled water,
p
DL
= 15 ng ofSb
';b'
::s
a) HG-GC -AAS
a) S-C
a) Helium
(CH,),SbCI, (100-200 ng), sample (0.1-3 mil. pH 0.51
a) HG and trapping on column
= 3 min a) No rearrangement at pH 6.10-6.76, reKoch et al. 1998
5b) HG-CTb) B
b) Helium
to 6.76 using various acids and buffers, 2% w/v NaBH,
b) Reaction mixture purged
= 6 min
arrangement at pH 0.51-3.30 (max
= 24%),
'"
ICP-MS
80ml min- 1
b) de-ionised water (10 mil, (CHl)lSbCI, (1 ng),
CO/acetone trap used
sample matrix affects rearrangement,
p
1 M HCI (re-distilled), 6% w/v NaBH, (0.8 ml)
DL
= 4 ng; b) pH similar results to a)
:-tI
max. rearr. 68%, DL
= 0.01 ng
~
HG-CT-AAS
Helium
In millipore-Q water (53 mll.acetic acid (3 mil,
Purged and collected on (old trap
Jenkins et al.
~
' "'
40 ml min- 1
trimethylantimony standard (4.9 ~I),
NaBH, (10 mg)
1998b,(
~
HG-CT-ICP-MS
Helium
Sample (1 g), bidistilled H,O (5 mil. HCI, pH 2
Degassing(l min), purging (10 min)
Rearrangement not reported
Krupp et al. 1996
0
400 ml min- 1
5% NaSH, (1.5 mil
'"
or
HG,
6% m/m NaBH, (purged with H, for 30 min) (0.5 ml)
Conducted in a sealed vial (15 ml)
No rearrangement reported, only
Feldmann et al.
::r
a) GC-ICP-MS
(CHl)lSbCI, (30 ng as Sb), deionised water(l mil, pH 7
injected onto column using a
trimethylantimony detected
1998
t-'
b) GC-MS-MS
Helium
gas-tight syringe
~
a) Sample (4 mil. 0.05 M citrate buffer pH 6, 2% NaSH,
en
a) HG-GC-AAS
a) S-C
Helium
b) Degassing (1 min), purge and
a) and b) No rearrangement seen
Andrewes et al.
3
b) HG-GC-ICP-MS b) B
70 ml min- 1
b) water (10 ml), 6% NaSH, (0.8 ml)
trapping (6 min) column in liq. N,
1998
s:
HG-CT-GCHelium
Sample (condensed water) (10 mil. 5% NaBH, (1 ml),
Degassing (10 min)
No rearrangement reported
Feldmann et al.
~
-1
ICP-MS
500 ml min, degassing pH 2 acidified with 1 M HCI (1.5 ml)
1994
?>
100 ml min purging
s::
0
' "'
::l.
'"