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#106
Optimizing Standard PreparationAnne Jurek
Optimizing Standard Preparation
human e
Discuss
analysis from watcarryove
large am
that sam
no longe
This app
The sam
volume.
Abstractt:
Standardd preparatio
linearity aamatrix staa
ion:
There haain the past ter manager.
concentrrator, the abi
Environmmounts of mental labor
follow staa
among thhese standapreparatii
procedurrooaltered t lication not
curve lineearity and c
Experimmental:
pling systeand Encoo
Coupled to The GC wwas configuparametee
nn can often rror or inconnnd/or continnndard prepp
ve been maa
mment to limitiHowever,, in creating
lity of the ceethanol has
ndard operaaple handlingg
on. Since nndle larger r able to hann
es for standdard preparaccommoddate the con
ee will exploroompound re
mm used for tn Evolutionn
the samplinred with a
rs for both tt
sistencies bbtion reproduing calibraa
aration techh
ny advanceeen years. TThese impro
ng the amo
ooncentrator tbbecome an iequired to aatories are r
ting proceddures in ord and analyssis is consistrd operatinggew purge ann
aation may necentrator’s l
ee how methsponse.
concentratoor. The exp
RRestek Rtx-6he purge ann
bbe a time coonsuming, tetween indii
ucibility. Thniques for UUSEPA Met
s in purge aand trap vvements vauunt of sampl
a more efficcient o tol ratessue.
wwrite and eer to prove ent. Chief
proceduressd trap concc
aamounts mettentrators arrhanol, the ed to be imitations.
aanol affects
hhis study wass the EST
g system weere an Agile24 20m x 0.
d trap and GGC/MS are
vidual prepaaration techis applicati
hhod 8260b.
rry e
is standardd e
eriments weere run in wnt 7890A G180mm x 1.
listed in Ta
eedious proceess. The opnniques can i
oon note will
AAnalytical Ceenturion WSaater mode CC and 59750µm colum
bbles 1 and 2
pportunity for nhibit curve
eexplore wat
autosamplwwith a 5mL p inert XL Mnn. respectivel
eer
eer uurge
SS. Experi eental
yy.
i n s p i r a t i o n m e e t s i n n o v a t i o n !
M
Ov
Purge an
ValTran
oisture Redu
DrDesorb
De
DMoistt
Sparge
Purge an
Internal
Inleet Head PresMode
Split Ratio
Column
Coolumn Flow Gas
Total Flow Source TemQuad Temp
MS TTransfer LineScan Rang
Scans Solvent Dela
Trap Type vve Oven Tem
TTrap Temp. cction Trap (PPurge Time PPurge Flow
Dryy Purge Flow
Pressure Cssorb Pressur
DDesorb Time eesorb Temp.
ure Reductioon Trap (MoBBake Temp VVessel Bake BBake Time Bake Flow
SSample Size Standard V
Tabble 1: Purg
GC/MS Inlet
Inlet Temp. ssure
een Temp. Proggram
RRate
pp. . Temp. ee
y
Table 2:
dd Trap Conceentrator
pp. ssfer Line Temmp.
MMoRT) Temp.
yy Purge TemppDr .
yy Purge Time oontrol ee
RRT) Bake Te
TTemp.
dd Trap Auto-SSampler
oolume
ee and Trap
Agilent
445ºC hold for 2200ºC, hold for
GGC/MS Para
ESE
Vo
1
1
mmp.
EST C
77890A/5975 SSplit/Splitless
200ºC 20.198 psi
Split 40:1
Rtx-624 20mm x 0.18mm I.thickness
00.3 min., 11.0.8mL/min
Helium 35.8mL/min
230ºC 150ºC 180ºC
3..0.7 min
meters
TT Encon vvolution ccarb 3000 1130ºC 1130ºC 35ºC 39ºC
111 min. 400mL/min aambient
400mL/min .0 min.
On 12psi .0 min. 2260ºC 2230ºC 2260ºC 1110ºC
8 400mL/min
eenturion WS 5mL 5µL
PParameterss
iinert XL
D. 1µm film
1 min., rampp 18ºC/min to
m/z 35-26512 scans/secc
002 min. runtimme
i n s p i r a t i o n m e e t s i n n o v a t i o n !
standard
in Table
%Methano
*%Methan
establis
versus pmethano
The USEEPA Methodconcentrration was 2was at 100
s was calcuthat the mm
3.percent mmconcentrrations.
Methanol inn 200ppb Cal
IS Methanool
Size Sampple
Standard aand IS Metha
l in Purged S
Standaard Concentr
0.5ppb to
20ppb to 2200ppb cal.
A nine pooint calibraticalibratioon curve pre
calibratiooeercent methl results we
needed tto be linear
8260b stan
,000µg/ml aa
aximum ammStandardd
ethanol diffferences se
Standard
nnol
ample
aations
10ppb cal. sttandards
sstandards
ol includes thh
Tablle 4: Stock
hh the curve aan of the anaa
anol in the rre excludedrregressed a
dards were0000µg/ml forr all of the a
nd p&m-xyylene which lated using tthe 200ppb ount of meethanol was
s were preppared at two
1µl/ml
1µl/ml
5ml
0.2%
Tablee
0.2% MMethanol
20ppm
200ppm
e added methhanol from th
oon curve waas preparedparation is ppresented in nd Agilent CChemstationlytes. The aanalytes we
sstandards; t from the rennd still the r
purchased nnalytes with wwas at 400calibration
en when pree
in this standddifferent cooparing a cu
%Methaa
2µl/ml
1µl/ml
5ml
10µl/5mml 15µl/5ml
0.3%
3: Percennt Methano
Standaa
0.3% MMethanol
10ppm
1100ppm
Standard PP
re also exahhese results ssults table deesults were
ffrom Restek
00µg/ml. The sstandard as ard. Thesencentrationrve. Refer
nol Calculattion
5µl/ml
1µl/ml
5ml
30µl/5ml
0.6%
ll Calculatio
rd Preparatiion
0.6% MMethanol M
4ppm
440ppm
e internal staandard
reparation
and run for eeach perceTable 5. AA range of 0. software waas employe
mmined to estare listed i
uue to the fannot linear to
. The comthe exceptioon of tert-b
percent mea reference calculationss in order to
10µl/ml
1µl/ml
5ml
555µl/5ml
1.1%
n
1.1% ethanol
22ppm
220ppm 1
for Calibraa
nnt methanol
dd to ascertaablish com
nn Table 6. Tcct that all of 200ppb.
ppound uutyl alcohol thanol in th due to the fss are displaminimize th
tto Table 4 foor standard
220µl/ml0
11µl/ml 1
5ml
1005µl/5ml
2.1%
22.1% Meethanol
11ppm
0ppm
tion Curvess
level. The 5 to 200ppbb was used t
iin the linear ppound respohe 5.1% tthe compou
wwhich ee aact yyed e
µ 00µl/ml
µl/ml
5ml
2555µl/5ml
55.1%
55.1% Meethanol
4000ppb
44ppm
o
nse
nds
i n s p i r a t i o n m e e t s i n n o v a t i o n !
**
Calibration SStandard Concentrration
0.5pppb
1ppbb
2ppbb
5ppbb
10ppbb
20ppbb
50ppbb
100pppb
200pppb
All standardd
0.2% Methanol
2.5µl 220ppm std.
5µl 220ppm std.
10µl 220ppm std.
25µl 220ppm std.
50µl 220ppm std.
10µl 2000ppm std.
25µl 2000ppm std.
50µl 2000ppm std.
100µl 2000ppm std.
s diluted in DD
0.3% Methanol
5µl 10ppm std.
10µl 10ppm std.
20µl 10ppm std.
50µl 10ppm std.
100µl 10ppm std.
20µl
50µl
100µl
200µl 100ppm std
e-ionized waa
Tablee
Calibrationn Curve Pre
0.6% Methan
12.5µl 4ppm st
25µl 4ppm st
50µl 4ppm st
125µl 4ppm st
250µl 4ppm st
100ppm std..50µl
40ppm s
100ppm std..125µl
40ppm s
100ppm std..250µl
40ppm s
..500µl
ter into a 1000
5: Calibraa
pparation
ool
dd. 2ppm
dd. 2ppm
dd. 2ppm
dd. 2ppm
dd. 2ppm
ttd. 20ppm
ttd. 20ppm
ttd. 20ppm
40ppm sttd. 1m
20ppm
ml volumetricc flask.
tion Curvee Preparati
1.1%% Methaanol
25µµl std.
5
50µµl std.
1
100µµl std.
2
250µµl std.
5
500µµl std.
1
100µµl std.
2
250µµl std.
5
500µµl std.
1
l std.
oon
2..1% Metthanol
0µl 1ppmm std.
000µl 1ppmm std.
000µl 1ppmm std. 4
000µl 1ppmm std.
ml 1ppmm std.
000µl 10pppm std. 4
000µl 10pppm std.
ml 10pppm std.
22ml 10pppm std.
5.1% MMethanol
125µl 4000ppb std.
250µl 4000ppb std.
500µl pppb std.
11.25ml 4pppb std.
22.50ml 4pppb std.
500µl pppm std.
11.25ml 4pppm std.
22.50ml 4pppm std.
55.00ml 4pppm std.
i n s p i r a t i o n m e e t s i n n o v a t i o n !
Chloromet
Bromomet
1,1,2-trichl
Acetone
Methylene
MTBE
Ethyl Tert
2-Butanon
propionitril
THF
methyl acr
Tert Amyl
Benzene
propyl ace
Dibromom
CCompound
Dichlorodiffluoromethane
hane
Vinyl Chlorride
hane
Chloroethaane
Trichlorofluuoromethane
diethyl etheer
orofluoroethane
1,1-Dichlorroethene
Iodomethaane
Carbon Dissulfide
Carbon Dissulfide
Chloride
acetonitrilee
Tert Butyl AAlcohol
cis-1,2-Dicchloroethene
acrylonitrilee
Isopropylet
Vinyl acetaa
1,1-Dichlorr
trans-1,2-DDichloroethene
ethyl acetaate
2,2-Dichlorr
Bromochloo
e
opropane
romethane
methacryloo
e
nitrile
Chloroformm
ylate
Dibromofluuoromethane SUR
1,1,1-Trichhloroethane
2-Chloroetthylvinylether
Carbon Teetrachloride
1,1-Dichlorropropene
methyl aceetate
isobutyl alccohol
Methyl Ether
1,2-Dichlorroethane
tate
Trichloroetthene
1,2-Dichlorropropane
methyl methacrylate
ethane
Bromodichhloromethane
2-chloroethhanol 2-nitroproppane
Curve %RSD
6.10
9.88
7.23
8.64
8.20
2.88
3.68
5.71
5.42
11.10
13.31
10.55
4.56
8.72
8.65
9.01
3.75
5.43
12.01
7.23
8.71
5.05
her
te
oethane
Butyl Ether (ETBE)) 2.60
7.80
10.66
10.01
3.83
5.99
12.27
12.14
7.66
7.61
8.24
5.67
2.66
4.87
8.34
2.47
4.59
10.38
2.89
3.84
3.23
9.17
6.06
3.01
5.77
6.12
4.28
7.67 6.00
0.2% Methhanol
Ave. CCurve
RF
Curve %RSD
0.597 6.76
0.626 4.89
0.578 3.08
0.313 4.26
0.353 5.83
0.837 4.18
0.416 3.81
0.495 4.09
0.449 3.52
0.192 7.07
0.427 9.38
1.248 5.69
0.774 8.22
0.500 7.83
0.062 9.02
0.066 14.90
1.623 1.72
0.499 4.86
0.224 10.17
1.774 4.14
1.283 4.24
1.012 3.18
1.813 2.28
0.594 3.21
0.104 9.96
1.039 10.48
0.859 2.54
0.355 5.10
0.096 14.39
0.567 13.52
0.227 11.59
1.055 13.75
0.628 5.41
0.537 13.58
0.926 2.48
0.409 3.74
0.707 13.76
0.818 2.43
1.892 2.75
0.031 0.998*
1.771 2.74
2.330 2.52
0.826 2.28
0.630 4.39
0.378 2.40
0.354 4.57
0.302 3.50
0.213 2.70
0.281 1.98
0.154 7.48 0.144 11.49
0.3% MMethanol
Ave. Curve
RF %
0.440
0.456 4.
0.428
0.233 12
0.267
0.636
0.323
0.379 5.
0.347
0.127 14
0.370 10
0.934
0.577 6.
0.386
0.035 13
0.030 12
1.218
0.388
0.176
1.293
1.000
0.738
1.310 3.
0.440
0.077 11
0.790
0.635 2.
0.257
0.067 11
0.439 12
0.171
0.831
0.480
0.434
0.704 3.
0.319
0.521 13
0.617
1.424
0.014
1.291
1.716
0.620
0.451
0.265
0.247
0.223
0.157
0.200 4.
0.113 0.104 10
0.66% Methanol
Currve RRSD
Ave. Curve
RF
4.777 0.368
110 0.426
3.226 0.408
..02 0.247
3.666 0.265
4.557 0.625
5.224 0.331
005 0.383
3.448 0.350
..52 0.165
..79 0.365
8.669 0.919
558 0.597
6.004 0.387
..64 0.041
..82 0.045
2.881 1.266
3.119 0.384
9.556 0.197
4.449 1.344
2.881 1.060
2.773 0.764
449 1.340
2.882 0.442
..82 0.090
8.771 0.907
884 0.629
2.009 0.262
..56 0.075
..52 0.484
6.994 0.195
7.337 0.812
5.115 0.518
7.447 0.418
227 0.704
4.008 0.330
..79 0.526
2.222 0.618
2.449 1.515
0.9998* 0.021
3.554 1.334
2.333 1.751
1.889 0.636
3.882 0.513
2.882 0.282
3.008 0.261
3.334 0.243
3.996 0.168
662 0.217
7.009 0.118 ..58 0.117
Curve %RSD
Ave.
RF
11.00 0.197
11.74 0.245
7.99 0.239
11.75 0.145
7.74 0.160
5.36 0.378
5.42 0.194
8.96 0.225
4.61 0.204
11.53 0.092
7.56 0.211
6.70 0.512
4.71 0.348
9.75 0.237
7.54 0.026
13.76 0.022
3.56 0.745
9.17 0.236
9.54 0.110
4.86 0.791
9.25 0.616
4.85 0.447
2.68 0.805
7.60 0.275
8.21 0.050
13.64 0.535
9.12 0.354
5.30 0.161
11.03 0.040
10.01 0.280
8.92 0.110
9.59 0.497
4.49 0.294
14.23 0.272
3.47 0.430
7.86 0.195
10.18 0.320
4.69 0.382
2.73 0.911
8.15 0.009
3.57 0.817
1.99 1.066
4.85 0.394
5.97 0.316
3.04 0.178
2.97 0.164
6.18 0.150
3.82 0.105
4.05 0.135
13.25 0.078 7.52 0.064
1.1% Methanoll
Curvee Curve %RSD
11.54 0
9.76 0
7.55 0
0.995* 0
8.13 0
6.62 0
2.84 0
6.74 0
6.84 0
0.995* 0
15.04 0
12.70 0
7.39 0
12.90 0
9.08 0
0.998* 0
2.99 0
10.65 0
6.28 0
4.89 0
7.18 0
5.70 0
2.45 0
7.15 0
11.27 0
0.998* 1
5.36 0
9.51 0
6.37 0
8.07 0
13.30 0
9.83 0
5.29 0
14.00 0
5.34 0
4.36 0
10.58 0
6.95 0
3.35 0
14.64 0
3.85 0
4.92 1
9.43 0
4.19 0
6.65 0
3.8 0
6.42 0
5.31 0
3.93 0
8.51 011.15 0
2.1% Methaanol
AAve. Cuurve
RRF
..255
..289
..266
..143
..166
..389
..202
..227
..215
..402
..202
..556
..361
..246
..031
..038
..764
..246
..116
..797
..576
..460
..818
..284
..053
..053
..324
..172
..042
..284
..116
..504
..313
..277
..433
..208
..328
..392
..915
..010
..825
..109
..414
..309
..181
..161
..153
..108
..130
..074
..062
i n s p i r a t i o n m e e t s i n n o v a t i o n !
Toluene
ethyl meth
Chloroben
Styrene
Xylene (o)
Isopropylb
cis-1,4-dic
BFB SUR
Bromoben
sec-Butylb
Naphthale
Average
*
CCompound
cis-1,3-Dicchloropropene
4-methyl-22-pentanone
Toluene-d88 SUR
acrylate
trans-1,3-DDichloropropene
1,1,2-Trichhloroethane
Tetrachlorooethene
1,3-Dichlorropropane
isopropyl aacetate
butyl acetaate
Dibromochhloromethane
2-Hexanonne
1,2-Dibrommoethane
zene
1,1,1,2-Tettrachloroethane
Ethylbenzeene
Xylene (m++p)
n-amyl aceetate
Bromoformm
enzene
hloro-2-butene
1,2,3-Trichh
zene
loropropane
1,1,2,2-Tettrachloroethane
n-Propylbeenzene
trans-1,4-ddichloro-2-butene
2-Chlorotool
4-Chlorotool
uene
uene
1,3,5-Trimee
tert-Butylbee
pentachlorr
thylbenzene
nzene
oethane
1,2,4-Trimee
enzene
thylbenzene
nitrobenzeene
1,3-Dichlorrobenzene
1,4-Dichlorr
Isopropyltoo
1,2,-Dichloo
n-Butylbenn
1,2-Dibromm
1,2,4-Trichh
obenzene
luene
robenzene
zene
o-3-chloropropanee
lorobenzene
Hexachloroo
ne
butadiene
1,2,3-Trichhlorobenzene
Linear Reegression Value
Curve %RSD
3.13
6.49
3.41
3.80
4.01
4.61
3.29
6.73
2.93
6.50
4.48
6.27
5.04
5.30
5.66
3.89
3.75
4.02
5.03
4.32
3.70
8.78
5.01
8.18
10.69
5.97
3.57
6.44
3.05
6.87
4.22
4.54
2.70
2.80
9.48
3.27
4.20
8.91
5.52
8.12
3.75
4.87
4.31
8.86
4.50 8.98
5.07
7.84
6.15
0.2% Methhanol
Ave. CCurve
RF
Curve %RSD
0.581 2.53
0.432 5.00
1.292 3.33
0.899 2.70
0.542 5.75
0.565 6.16
0.322 2.88
0.357 6.97
0.569 2.09
0.097 1.69
0.279 4.18
0.358 8.32
0.307 8.80
0.331 2.72
1.118 1.78
0.376 6.68
1.964 2.54
3.096 3.23
1.242 3.59
1.566 3.38
0.850 2.24
0.273 11.04
1.945 3.8
0.189 12.37
1.051 4.73
1.379 3.43
1.183 4.66
0.909 3.72
4.183 2.02
0.327 5.76
0.788 2.12
0.824 1.79
2.832 2.95
2.430 2.63
0.360 8.07
0.732 3.76
2.917 2.97
0.077 11.32
1.558 2.32
1.620 5.59
3.001 4.36
1.510 1.845
2.643 3.83
0.204 7.93
0.945 3.02 3.167 4.73
0.334 11.38
0.903 2.55
0.907 5.40
0.3% MMethanol
Ave. Curve
RF
0.406
0.300
0.895
0.639
0.384
0.383
0.232
0.231 8.
0.408
0.071 10
0.198
0.249
0.220
0.240
0.738
0.250
1.322
1.027
0.829
1.035 2.
0.567
0.186 13
1.292
0.126 12
0.667
0.880
0.785
0.617
2.707
0.221
0.514
0.535
1.805
1.558
0.285
0.469 2.
1.865
0.029 14
1.018
1.072
1.915
0.992
1.722
0.135
0.633 2.097
0.237
0.600
5.0.619
Table 6:: Data Sum
0.66% Methanol
Currve %RRSD
Ave. Curve
RF
4.666 0.419
5.224 0.353
4.663 0.942
2.554 0.679
4.336 0.421
5.776 0.404
2.440 0.246
996 0.243
2.991 0.430
..40 0.077
2.992 0.221
9.440 0.265
7.111 0.263
2.449 0.258
3.779 0.744
6.669 0.248
2.338 1.323
2.556 1.027
4.448 0.818
002 1.036
3.775 0.588
..72 0.184
4.119 1.279
..50 0.127
7.001 0.631
5.006 0.846
4.003 0.779
3.338 0.603
2.554 2.551
6.554 0.225
3.551 0.487
2.777 0.509
3.007 1.717
2.996 1.475
6.774 0.272
442 0.449
2.776 1.778
..98 0.031
2.889 0.947
9.000 1.019
4.446 1.818
3.338 0.930
4.110 1.618
7.002 0.135
8.222 0.608 2.222 2.056
5.440 0.211
4.115 0.570
660 0.619
mmary
Curve %RSD
Ave.
RF
5.07 0.262
4.83 0.213
2.47 0.623
2.97 0.435
5.69 0.261
6.96 0.249
3.74 0.158
9.42 0.160
1.98 0.278
8.93 0.049
6.21 0.137
11.76 0.163
5.05 0.153
2.92 0.163
6.39 0.555
7.26 0.178
2.55 0.963
3.02 0.756
4.47 0.592
2.96 0.757
6.81 0.408
14.76 0.129
3.16 0.933
0.999* 0.081
10.72 0.528
4.64 0.664
6.86 0.581
4.5 0.462
2.99 2.033
6.55 0.158
2.57 0.386
3.38 0.406
3.34 1.352
3.02 1.176
0.997* 0.199
2.98 0.352
2.92 1.395
0.997* 0.016
5.94 0.764
11.54 0.818
3.89 1.437
4.16 0.739
6.08 1.257
10.46 0.096
4.12 0.458 5.48 1.528
7.45 0.161
4.21 0.428
6.50 0.422
1.1% Methanoll
Curvee Curve %RSD
6.75 0
7.31 0
5.23 0
4.96 0
5.99 0
8.28 0
5.36 0
4.67 0
3.97 0
6.58 0
4.98 0
13.39 0
10.98 0
4.73 0
8.40 0
9.29 0
4.32 0
4.88 0
5.25 0
3.52 0
7.01 0
14.61 0
4.22 0
0.997* 0
14.71 0
9.88 0
4.59 0
3.39 0
4.21 1
5.10 0
5.77 0
10.01 0
3.99 1
4.67 1
9.08 0
7.23 0
4.56 1
14.74 0
13.10 0
7.56 0
5.63 1
7.02 0
7.05 1
7.87 0
12.11 05.75 1
14.66 0
8.93 0
7.52 0
2.1% Methaanol
AAve. Cuurve
RRF
..253
..213
..611
..426
..251
..244
..154
..143
..274
..046
..130
..157
..156
..161
..539
..169
..931
..734
..579
..722
..367
..117
..899
..076
..509
..657
..556
..446
..940
..143
..374
..402
..305
..130
..216
..339
..349
..015
..771
..768
..375
..719
..225
..091
..465
..499
..170
..437
..427
i n s p i r a t i o n m e e t s i n n o v a t i o n !
Figuree
Figure
1: Overlayy
2: Overlayy
of Bromoff
of 50ppb SS
orm Respoonse Ion 172.1%%
tandard ChhromatogrMMethanol
Methanol)) 33 (Blue plott
aams with 0.22
0.2% Methh
% (Blue) aa
anol, Red pplot
nd 2.1% (RRed)
i n s p i r a t i o n m e e t s i n n o v a t i o n !
Compou
standard
methano
Conclussion:
The Encoon Evolutiond respons
Bromoforrm responss.
5.1% meethanol lineamuch forr the system
calibratiooillustratioo
nn proved to
Curve linnrity could nto handle a
l for better reen standardss produced t
methanol rn with 0.2%
ees passed fooee decreased earity was cc
nd the recosults. It shhould be not
he optimumeefer to App
bbe an excelleent system r all of the SSPCC compdramaticallyy with the inonsistent thh
oot be achieveed. Overall, mmmendatio
compound eendix A.)
ffor handling oounds up tocreased pe
rough the sttudy up to 25.1% meth
eed that the loower the mresponses.
large amou
rrcent of met.1% metha
aanol in the soonn would be t introduce leethanol volu (For a stan
nnts of meth 2.1% methaanol, but th
hhanol in the
mme in the ddard prepar
aanol. ee
nnol; howeverr at ttandards waas too ess than 2%%
aation
i n s p i r a t i o n m e e t s i n n o v a t i o n !
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