JSB is an authorised partner of...ndard prepp ve been maa mment to limiti However,, in creating lity of the c eethanol has ndard operaa ple handlingg on. Since nn r able to hanndle

JSB is an authorised partner of

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 !

#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.


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


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


**

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.


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


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


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)


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


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Documents

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