Assessment of the precision and accuracy of laser ablation-ICPMS
analyses in the Fluids Research Laboratory within the Department of
Geosciences, Virginia Tech, Blacksburg, VA U.S.A.
The following document describes results of laser ablation ICP-MS analyses of several
standards of known composition conducted using the LA-ICPMS system installed in the
Department of Geosciences at Virginia Tech to evaluate the precision and accuracy of
analyses. The values reported here apply in general to analyses of solid materials in
which ablation starts at the sample surface, and do not necessarily apply to analyses of
fluid inclusions where the accuracy and precision are related to inclusion size and depth
beneath the surface, among other factors.
To asses the accuracy and precision of analyses, NIST standard 610 was used as the
reference, and then each of several other standards were analyzed as “unknowns”.
Accuracy was assessed by comparing the elemental abundances predicted by our
analyses with the “known” values. Each standard (USGS standards BCR-2G, BHVO-2G,
BIR-1G, NKT-1G and NIST standards NIST612 and NIST614) was analyzed five times
according to the specifications indicated in Table 1.
USGS standards BCR-2G, BHVO-2G and BIR-1G are natural basalt glasses
distributed by the USGS. NKT-1G is a natural nephelinite glass distributed by the USGS
(http://crustal.usgs.gov/geochemical_reference_standards/basaltbcr2.html). NIST 612 and
614 are commercial standard reference materials obtained from the National Institute of
Standards and Technology.
The data were reduced using the AMS software (Mutchler et al., 2008), using NIST610
glass as external standard and assuming that the elements analyzed represent 100 % of
the sample (as oxides). The average concentration in ppm, average limit of detection in
ppm, standard deviation in ppm and number of analyses above the detection limit (n) of
the 5 analyses for each element are reported in Table 2.
The precision of the measurements is reported as percent relative standard deviation
(%RSD) for each element, which is calculated as the standard deviation divided by the
average concentration. The %RSD provides an estimate of the consistency of the
analyses of the same standard, or in other words, the reproducibility of the measurement.
1
The relative standard deviation is mostly within 5-10 percent (Fig. 1) indicating that
repeated analyses of the same material give results that are consistent to within 5-10 %.
The accuracy of the measurement is reported as the average percent error for each
element, and is calculated as the average of the differences between each individual
analysis and the known concentration for the standard. The known concentrations used to
evaluate the accuracy of the LA-ICPMS analyses are the preferred concentrations in the
standards reported by the Max-Plank-Institut für Chemie at http://georem.mpchmainz.gwdg.de. The average percent error provides an estimate of the difference between
the calculated and known concentration. The average percent error is mostly within 515% (Fig. 2) indicating that the measured concentrations agree with the known
concentrations within 5-15 %.
Mutchler SR, Fedele L & Bodnar RJ (2008) Analysis Management System (AMS) for
reduction of laser ablation ICPMS data. In Laser-Ablation-ICPMS in the Earth
Sciences: Current Practices and Outstanding Issues (P. Sylvester, ed.) Mineralogical
Association of Canada Short Course Series, Vol. 40, 318-327.
The following data are the result of work conducted in the LA-ICPMS laboratory in
the Department of Geosciences, Virginia Tech, Blacksburg, VA. These data are
provided as a mean to evaluate the basic analytical performance of our laboratory.
Please reference this report in your publications using this link:
http://www.geochem.geos.vt.edu/fluids/laicpms/VT_LAICPMS_Accuracy_Precision
.pdf.
If you use this site as a reference for the accuracy and precision of your data, please
email the information regarding your publication to Dr. Robert Bodnar
(rjb@vt.edu).
Raw data are available upon request. Please email Luca Fedele (lfedele@.vt.edu)
2
LA−ICPMS instrument and data acquisition parameters
Excimer 193−nm ArF laser GeoLasPro
Output Energy
150 mJ
Energy Density on sample
~ 7 − 10 J/cm2
Repetition Rate
5 Hz
Pit Size
Between x and x µm
Ablation Cell Volume
~ 1.5 cm3
Cell Gas Flow (He)
~ 1 L/min
Agilent 7500ce quadrupole ICP−MS
Auxiliary gas flow
RF power
Detector Mode
Quadrupole Settling Time
Data acquisition parameters
Sweeps per reading
Reading per replicate
Replicates
Dwell time per isotope
Points per peak
External Standard
Spot size
Isotopes Analyzed
1.03 l/min Ar
1500 V
Dual 8 orders of magnitude linear dynamic range
2 ms
1
200 − 300
1
10 ms
1 per measurement
NIST610 glass
60 µm
Li (7), Be (9), B (11), Na (23), Mg (25), Al (27), Si (28),
K (39), Ca (40), Sc (45), Ti (49), V (51), Cr (52), Mn (55),
Fe (56), Co (59), Ni (62), Cu (63), Zn (66), Ga (69), As
(75), Rb (85), Sr (88), Y (89), Zr (90), Nb (93), Ag (107),
Sn (120), Sb (121), Cs (133), Ba (138), La (139), Ce
(140), Pr (141), Nd (143), Sm (147), Eu (153), Gd (157),
Dy (163), Er (166), Yb (172), Lu (175), Hf (178), Ta
(181), Au (197), Pb (208), Th (232), U (238)
3
RSD %
0.0
5.0
10.0
15.0
20.0
25.0
30.0
35.0
40.0
45.0
50.0
BCRT2G
BHVOT2G
BIRT1G
NISTT612
NISTT614
NKTT1G
Li*(7)
Be*(9)
B*(11)
Na*(23)
Mg*(25)
Al*(27)
Si*(28)
K*(39)
Ca*(40)
Sc*(45)
Ti*(49)
V*(51)
Cr*(52)
Mn*(55)
Fe*(56)
Co*(59)
Ni*(62)
Cu*(63)
Zn*(66)
Ga*(69)
As*(75)
Rb*(85)
Sr*(88)
Y*(89)
Zr*(90)
Nb*(93)
Ag*(107)
Sn*(120)
Sb*(121)
Cs*(133)
Ba*(138)
La*(139)
Ce*(140)
Pr*(141)
Nd*(143)
Sm
Eu*(153)
Gd*(157)
Dy*(163)
Er*(166)
Yb*(172)
Lu*(175)
Hf*(178)
Ta*(181)
Au*(197)
Pb*(208)
Th*(232)
U*(238)
Precision
Fig. 1 - Precision of the analyses reported as relative standard deviations (RSD %) for each of the elements
that had concentrations above LOD in standards BCR-2G, BHVO-2G, BIR-1G, NKT-1G,
NIST612 and NIST614. The blue area corresponds to an RSD of <5 %, and the red box
corresponds to RSD ≤10 %.
4
Average % Error
!40.0
!30.0
!20.0
!10.0
0.0
10.0
20.0
30.0
40.0
BCR!2G
BHVO!2G
BIR!1G
NIST!612
NIST!614
NKT!1G
Li*(7)
Be*(9)
B*(11)
Na*(23)
Mg*(25)
Al*(27)
Si*(28)
K*(39)
Ca*(40)
Sc*(45)
Ti*(49)
V*(51)
Cr*(52)
Mn*(55)
Fe*(56)
Co*(59)
Ni*(62)
Cu*(63)
Zn*(66)
Ga*(69)
As*(75)
Rb*(85)
Sr*(88)
Y*(89)
Zr*(90)
Nb*(93)
Ag*(107)
Sn*(120)
Sb*(121)
Cs*(133)
Ba*(138)
La*(139)
Ce*(140)
Pr*(141)
Nd*(143)
Sm
Eu*(153)
Gd*(157)
Dy*(163)
Er*(166)
Yb*(172)
Lu*(175)
Hf*(178)
Ta*(181)
Au*(197)
Pb*(208)
Th*(232)
U*(238)
Accuracy
Fig. 2 - Accuracy of the analyses reported as the average percent error for each of the elements that had
concentrations above LOD in standards BCR-2G, BHVO-2G, BIR-1G, NKT-1G, NIST612 and
NIST614. The blue area corresponds to an average percent error of ±5 %, and the red box
corresponds to an average percent error of ±15 %.
5
Measured / STD
,',
(3)
(5)
(--)
(./)
(.1)
(.3)
(.4)
(/5)
(0,)
(01)
(05)
(1-)
#(1.)
!(11)
(12)
"(15)
(2.)
%(2/)
!(22)
(25)
$(31)
(41)
#(44)
(45)
#(5,)
(5/)
(-,3)
!(-.,)
(-.-)
$(-//)
(-/4)
(-/5)
(-0,)
#(-0-)
(-0/)
(-03)
%(-1/)
(-13)
&(-2/)
#(-22)
(-3.)
%(-31)
(-34)
(-4-)
%(-53)
(.,4)
(./.)
(./4)
,'.
,'0
,'2
,'4
-',
-'.
-'0
-'2
-'4
.',
Fig. 3 – Ratios of Measured over reference values for USGS Basaltic glass BCR-2G. Shaded area
represents ±10% variation. Red box represents ±20% variation. Reference values are from
GeoReM (http://georem.mpch-mainz.gwdg.de/). Some ratios were not plotted either because the
element was not detected or a reference value was not available (cfr. Table 1).
6
Measured / STD
,',
(3)
(5)
(--)
(./)
(.1)
(.3)
(.4)
(/5)
(0,)
(01)
(05)
(1-)
#(1.)
!(11)
(12)
"(15)
(2.)
%(2/)
!(22)
(25)
$(31)
(41)
#(44)
(45)
#(5,)
(5/)
(-,3)
!(-.,)
(-.-)
$(-//)
(-/4)
(-/5)
(-0,)
#(-0-)
(-0/)
(-03)
%(-1/)
(-13)
&(-2/)
#(-22)
(-3.)
%(-31)
(-34)
(-4-)
%(-53)
(.,4)
(./.)
(./4)
,'.
,'0
,'2
,'4
-',
-'.
-'0
-'2
-'4
Fig. 4 – Ratios of Measured over reference values for USGS Basaltic glass BHVO-2G. Shaded area
represents ±10% variation. Red box represents ±20% variation. Reference values are from
GeoReM (http://georem.mpch-mainz.gwdg.de/). Some ratios were not plotted either because the
element was not detected or a reference value was not available (cfr. Table 1).
7
Measured / STD
,',
(3)
(5)
(--)
(./)
(.1)
(.3)
(.4)
(/5)
(0,)
(01)
(05)
(1-)
#(1.)
!(11)
(12)
"(15)
(2.)
%(2/)
!(22)
(25)
$(31)
(41)
#(44)
(45)
#(5,)
(5/)
(-,3)
!(-.,)
(-.-)
$(-//)
(-/4)
(-/5)
(-0,)
#(-0-)
(-0/)
(-03)
%(-1/)
(-13)
&(-2/)
#(-22)
(-3.)
%(-31)
(-34)
(-4-)
%(-53)
(.,4)
(./.)
(./4)
,'.
,'0
,'2
,'4
-',
-'.
-'0
-'2
-'4
.',
.'.
.'0
.'2
.'4
/',
Fig. 5 – Ratios of Measured over reference values for USGS Basaltic glass BIR-1G. Shaded area represents
±10% variation. Red box represents ±20% variation. Reference values are from GeoReM
(http://georem.mpch-mainz.gwdg.de/). Some ratios were not plotted either because the element was
not detected or a reference value was not available (cfr. Table 1).
8
Measured / STD
,'0
(3)
(5)
(--)
(./)
(.1)
(.3)
(.4)
(/5)
(0,)
(01)
(05)
(1-)
#(1.)
!(11)
(12)
"(15)
(2.)
%(2/)
!(22)
(25)
$(31)
(41)
#(44)
(45)
#(5,)
(5/)
(-,3)
!(-.,)
(-.-)
$(-//)
(-/4)
(-/5)
(-0,)
#(-0-)
(-0/)
(-03)
%(-1/)
(-13)
&(-2/)
#(-22)
(-3.)
%(-31)
(-34)
(-4-)
%(-53)
(.,4)
(./.)
(./4)
,'2
,'4
-',
-'.
-'0
-'2
-'4
.',
Fig. 6 – Ratios of Measured over reference values for USGS Nephelinite glass NKT-1G. Shaded area
represents ±10% variation. Red box represents ±20% variation. Reference values are from
GeoReM (http://georem.mpch-mainz.gwdg.de/). Some ratios were not plotted either because the
element was not detected or a reference value was not available (cfr. Table 1).
9
Measured / STD
,'0
(3)
(5)
(--)
(./)
(.1)
(.3)
(.4)
(/5)
(0,)
(01)
(05)
(1-)
#(1.)
!(11)
(12)
"(15)
(2.)
%(2/)
!(22)
(25)
$(31)
(41)
#(44)
(45)
#(5,)
(5/)
(-,3)
!(-.,)
(-.-)
$(-//)
(-/4)
(-/5)
(-0,)
#(-0-)
(-0/)
(-03)
%(-1/)
(-13)
&(-2/)
#(-22)
(-3.)
%(-31)
(-34)
(-4-)
%(-53)
(.,4)
(./.)
(./4)
,'2
,'4
-',
-'.
-'0
-'2
-'4
.',
Fig. 7 – Ratios of Measured over reference values for NIST glass NIST612. Shaded area represents ±10%
variation. Red box represents ±20% variation. Reference values are from GeoReM
(http://georem.mpch-mainz.gwdg.de/). (cfr. Table 1).
10
Measured / STD
,'0
(3)
(5)
(--)
(./)
(.1)
(.3)
(.4)
(/5)
(0,)
(01)
(05)
(1-)
#(1.)
!(11)
(12)
"(15)
(2.)
%(2/)
!(22)
(25)
$(31)
(41)
#(44)
(45)
#(5,)
(5/)
(-,3)
!(-.,)
(-.-)
$(-//)
(-/4)
(-/5)
(-0,)
#(-0-)
(-0/)
(-03)
%(-1/)
(-13)
&(-2/)
#(-22)
(-3.)
%(-31)
(-34)
(-4-)
%(-53)
(.,4)
(./.)
(./4)
,'2
,'4
-',
-'.
-'0
-'2
B (6.6)
Sc (55.6)
Fig. 8 – Ratios of Measured over reference values for NIST glass NIST614. Shaded area represents ±10%
variation. Red box represents ±20% variation. Reference values are from GeoReM
(http://georem.mpch-mainz.gwdg.de/). (cfr. Table 1).
11
Ga69$
Zn66$
Time (s)
40
60
80
100
120
Cu63$
Ni62$
Co59$
Fe56$
Mn55$
Cr52$
V51$
Ti49$
Sc45$
Ca40$
K39$
Si28$
Al27$
Mg25$
Na23$
B11$
Be9$
Li7$
1
10
100
1000
10000
100000
0
20
BHVO-2G
1000000
Counts
Fig. 9 – Typical example of LAICPMS signal collected on the USGS basaltic glass BHVO-2G (analyzed as
unknown). Shaded areas represent integration regions. Typically we select 50s for background
signal and 40s or more for sample signal.
(for more details: http://www.geochem.geos.vt.edu/fluids/laicpms/images/PosterWeb.pdf)
12
Table 1 – Data for Fig. 3 to 8
(3)
(5)
(--)
(./)
(.1)
(.3)
(.4)
(/5)
(0,)
(01)
(05)
(1-)
#(1.)
!(11)
(12)
"(15)
(2.)
%(2/)
!(22)
(25)
$(31)
(41)
#(44)
(45)
#(5,)
(5/)
(-,3)
!(-.,)
(-.-)
$(-//)
(-/4)
(-/5)
(-0,)
#(-0-)
(-0/)
(-03)
%(-1/)
(-13)
&(-2/)
#(-22)
(-3.)
%(-31)
(-34)
(-4-)
%(-53)
(.,4)
(./.)
(./4)
5
.'/
2
/'./
/'12
-/'0
10'0
-'35
3',2
//
.'.3
0.1
-3
,'.,
-.'0
/4
-/
.-.1
./
03
/0.
/1
-40
-.'1
,'1
.'2
,'/1
-'-2
24/
.0'3
1/'/
2'3
.4'5
2'15
-'53
2'32'00
/'3
/'/5
,'1,/
0'40
,'34
-1'5
-'25
$
&!
5'23,
-',30
.',/2
,'441
4'-42
-'/20
/'./1
-',,.
/'0.1
,'52.
-0'135
-',44
12'./0
-',/0
-'521
-',51
2'13/
,'5/1-'31.
-'124
.'-/5
,'50.
0,0'-0,'51-0'03,
,'41,'-41
,'5.2
--'/4/
,'5-4
/3'-,5
,'533
-5'-20
-'030
-4',04
,'415
-2-'-52
-'.5,
0-'303
-'4-1
,'5,3
1-',.-',42
/-.'3.0
,'5-0
.3'4.4
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-1-'.5.
,'4..
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,'433
,'21,
-'.55
-'522
,'312
,'02/
-'/./
-'-22
-',,2
204'200
,'51,
..'152
,'5-1
05'.,0
,'5./
1'53.
,'45.1'53/
,'455
1'3./
,'424
-'40/
,'5/2
1'300
,'412
1'/,1
,'4.0
.'51/
,'354
.'4.2
,'4/0
,'0,4
,'4-.
/'5-2
,'4,5
,'145
,'311
,',01
-,'5-.
,'55.
1'.-,'44/
-'2/4
,'525
$
&!
0'0
0'1.1
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-'/
,'542
,'314
5'-,/
.'0
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,'515
3'-/
2'524
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-0'353
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1-'-5/
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//
1,'3-2
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.'15.
,'5.5
/,4
/,-'/.5
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.5/
.3-'130
,'5.3
,'-3
,'-20
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--'/
-,'.01
,'5,3
00
00'10.
-',-.
--2
-.4'-2/
-'-,1
-.3
-.5'5,,
-',./
-,.
-..'-5-'-54
..
.1'52.
-'-4,
,'555
5'.
5'42/
-',3.
/52
/35',,.
,'513
.2
.,'5-.
,'4,0
-3,
-00',21
,'403
-4'/
-2'-4,'440
,'1.3
.'2
-'255
,'21/
,'/
,','--/
-'-.3
-/-.4'402
,'540
-1'.
-0'032
,'51.
/3'2
/1'2-1
,'503
1'/1
0'45,
,'5-0
.0'1
./'/.,'51.
2'1'152
,'5-3
.',3
-'524
,'512'-2
1'4,4
,'50/
1'.4
0'2-,
,'43/
.'12
.'-00
,'4/3
.',-'314
,'430
,'.35
,'.01
,'434
0'/.
/'3.5
,'42/
-'-1
,'415
,'303
,'/33
-'3
-'5/4
-'-0,
-'..
-'-,/
,'5,0
,'0,/
,'0,4
-',-.
/
,'-
-'41
5'0
-1'1
03'1
,',/
-/'/
0/
-',0
/.2
/5.
,'-5
-,'0
1.
-34
--5
34
-1
,'-53
-,5
-0'/
-0
,'1.
.'/
,'12
,',,3
2'1
,'2,5
-'45
,'/3
.'/3
-',5
,'1-3
-'41
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-'3
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,'.04
,'13
,',/2
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,',./
#
&!
/'.4.
-',50
,'.,.
.',./
3',5,
-'5,4
-',/5'.32
,'543
-2'1,0
-',21
04'520
-',/,',.1
,'40-.'040
,'5/5
12'1.3
-'/-1
,'441
,'41/,3'22/
,'500
/3-',25
,'503
,'-3,'455
5'142
,'5..
1/'45-',/2
-35'/,1
-',,3
-.4'212
-',444'1/.
-'-/1
-3'-4-'-01
,'033
.'0-5
-,/',,0
,'501
-.'025
,'43.
--'525
,'411
,'02/
,'45,
,'.0/
,'35/
,'/01
,'143
-',05
2'./5
,'52,
,'13,
,'5/2
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,'512
,'///
,'455
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,'5.5
,'52,
,'44,'03/
,'5-1
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,'421
.'-3,'41.
-'0.0
,'4/4
-'/51
,'41,'.-1
,'422
,'03/
,'4/,
,',/,'43/
,'0-2
/'24/
,'551
,',.2
,'415
,',/4
-'224
13
Table 1 – Cont.
(3)
(5)
(--)
(./)
(.1)
(.3)
(.4)
(/5)
(0,)
(01)
(05)
(1-)
#(1.)
!(11)
(12)
"(15)
(2.)
%(2/)
!(22)
(25)
$(31)
(41)
#(44)
(45)
#(5,)
(5/)
(-,3)
!(-.,)
(-.-)
$(-//)
(-/4)
(-/5)
(-0,)
#(-0-)
(-0/)
(-03)
%(-1/)
(-13)
&(-2/)
#(-22)
(-3.)
%(-31)
(-34)
(-4-)
%(-53)
(.,4)
(./.)
(./4)
'#$
&!
0,'.
0-'4/3
-',0/3'1
0.'23.
-'-/4
/0'/
/5'-30
-'-0.
-/'3
-/'1,/
,'542
24
2.'00.
,'5-4
.',/
.'.52
-'-/3.'3-'0/.
,'552.'/
2-'/.0
,'540
--'5
-.'1.1
-',1.
/5'5
3.'4.2
-'4.1
00
0,'4,0
,'5.3
/4'4
/4',-2
,'54,
/2'0
/1'21,
,'535
/4'3
/4'030
,'550
104'2-2
,'51/
/1'1
/0'40.
,'54/4'4
/3'./.
,'52,
/3'4
/2',.1
,'51/
/5'/5'-.4
-',,/2'5
/2'312
,'552
/1'3
/-'521
,'451
/-'0
/.',..
-',.,
34'0
4/'42/
-',3,
/4'/
0.'.42
-'-,0
/3'5
0.',.4
-'-,5
/4'5
/3'1/1
,'521
..
-5'5/3
,'5,2
/4'2
/0'1,,
,'450
/0'3
/-'-0,'453
0.'3
0,'315
,'511
/5'/
0-'2-3
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All elemental concentrations are in (ppm), except in RED -> %oxide [Na2O, MgO, Al2O3, SiO2, K2O, CaO,
FeO]. When the numbers for these elements are in blue then concentrations are expressed as elemental
(ppm) due to low amount. ND = Not detected; NR = Concentration not reported in the literature. All
reference concentration data are from GeoReM (http://georem.mpch-mainz.gwdg.de/). Avrg (5) = average
of 5 measurements. STD = Reference value
14
Table 2 - Basic Statistic: STDEV = Standard Deviation - %RSD = Relative Standard Deviation LOD =
Limits of Detection
!%
)4*
)6*
)..*
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)/2*
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)16*
)2.*
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&).20*
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6(34-(//2 /(0//
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315(311
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!%
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0(/5/
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0(-/2
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0(-21
0(.55
15
Table 2 – Cont.
!%
)4*
)6*
)..*
)/0*
)/2*
)/4*
)/5*
)06*
)1-*
)12*
)16*
)2.*
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1(2/2
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/06/63(4114/2(5244633(1.1
2-(4.3
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.(46.
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16
Table 2 – Cont.
!%
)4*
)6*
)..*
)/0*
)/2*
)/4*
)/5*
)06*
)1-*
)12*
)16*
)2.*
#)2/*
!)22*
)23*
")26*
)3/*
&)30*
!)33*
)36*
$)42*
)52*
#)55*
)56*
#)6-*
)60*
).-4*
!)./-*
)./.*
$).00*
).05*
).06*
).1-*
#).1.*
).10*
).14*
&).20*
).24*
').30*
#).33*
).4/*
&).42*
).45*
).5.*
&).64*
)/-5*
)/0/*
)/05*
.(114
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-(346
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6(51.
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0-(0/5
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15(60.(025 /(442
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/(5-4
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17
Table 3 – Color coded representation of the analytical variations presented in Table 1 (Measured/STD) and
in graphs 3 to 8.
2=3
2?3
2773
2893
28;3
28=3
28>3
29?3
2:63
2:;3
2:?3
2;73
%2;83
"2;;3
2;<3
#2;?3
2<83
*2<93
"2<<3
2<?3
&2=;3
2>;3
%2>>3
2>?3
%2?63
2?93
276=3
"27863
27873
&27993
279>3
279?3
27:63
%27:73
27:93
!27:=3
*27;93
27;=3
-27<93
%27<<3
27=83
*27=;3
27=>3
27>73
*27?=3
286>3
28983
289>3
&
#
76B
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86B
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76B
76B
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76B
86B
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86B
86B
76B
86B
86B
76B
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76B
76B
86B
76B
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86B
86B
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86B
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86B
86B
86B
86B
86B
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86B
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76B
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86B
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86B
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86B
76B
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& '
( &
" -( %%#%&# #%#0'%""'&C;B
+%(#"/ '- #,"'&C;176B+%(#"/ ' *
"'&C76186B+%(#"/ '$""'&+%(#"
#+C86B
18
Table 4 – Data for Fig. 1 and 2
19