100
NASA-CR-200776 _.,omract Ne. r,h, Sg-_8250-] 4 REPORT -. Finai Report Spacelab Charcoal _malyses - Phase 1I To Ion Electronics 6767 Madison Pike Hunts_dlle, At, 35806 January 20. 1995 vBallelle ... Pu*.ting Technology To"Work https://ntrs.nasa.gov/search.jsp?R=19960017611 2018-06-07T16:21:07+00:00Z

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Page 1: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

NASA-CR-200776_.,omract Ne. r,h, Sg-_8250-] 4

REPORT-.

Finai Report

Spacelab Charcoal

_malyses - Phase 1I

To

Ion Electronics

6767 Madison Pike

Hunts_dlle, At, 35806

January 20. 1995

vBallelle. . . Pu*.ting Technology To"Work

https://ntrs.nasa.gov/search.jsp?R=19960017611 2018-06-07T16:21:07+00:00Z

Page 2: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

I_I. WIT_: UIO0_ 02 SC2_S 21m TO IIWII/'I_ |4s3_m CfLI: ISSNICI_. 06 CUTOF 288 11) UIm_.Es Im PL _ S'rD lqlq_?_ TO Le;N..OI-I 2 nlMmm¢ S_..E55CC_S.s Wn X L32 I_ l.Rln I_ R'_ WSC:

G 1, I L.MELI H L. 4.8 _ it IL, L.o.J 0 BA_ U J, 3

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Page 3: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

...A.-- _j { _.

L

Final Report

Spacelab Charcoal Analyses- Phase II

to

ION Electronics

Contract No. NAS8-38250-14

January 20, 1995

by

L.E. Siivon, L.A. Hernon-Kenny,

V.R. Katona, L.E. Dejarme

BA'IWEI2_

505 King Avenue

Columbus, Ohio 43201-2693

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Page 5: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Introduction

This report describes analytical methods and results obtained from chemical analysis of

31 charcoal samples in five sets. Each set was obtained from a single scrubber used to filter

ambient air on board a Spacelab mission. Analysis of the charcoal samples was conducted

by thermal desorption followed by gas chromatography/mass spectrometry (GC/MS). All

samples were analyzed using identical methods. Two of the mission sample sets (IML,

USML) were analyzed previously by Battelle (Contract No. 38250-06) using a similar

method, however that method was unable to detect very volatile and/or very polar

compounds. The method used for these analyses was able to detect compounds independent

of their polarity or volatility.

In addition to the charcoal samples, Battelle was requested and authorized under

Contract Modification No. 5 to conduct analyses of three ECLSS water samples received on

December 15, 1994 specifically for trimethylamine.

Because of the number of samples and compounds identified, results from the charcoal

analyses are provided in Appendix A together with supporting GC./MS total ion

chromatograms. Results from Trimethylamine analyses on the three ECLSS water samples

are provided in the Results and Discussion section of this report.

Technical Approach

Charcoal Samples

Table 1 identifies the charcoal samples analyzed under this contract. As indicated

earlier, charcoal from the IML and USML missions was analyzed previously by Battelle and

was maintained in glass jars at room temperature from date of receipt. The charcoal type

shown in Table 1 was not indicated on the samples but was presumed by Battelle staff based

on the sample numbers, discussions with ION personnel and prior documentation received on

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on the sample numbers, discussions with ION personnel and prior documentation received on

charcoal samples. Also included in these analyses was a sample of clean activated charcoal

provided by Batmlle that was stored with the IML and USML samples from the date of

receipt. This "method blank" material is not identified in Table 1 but is represented in

subsequent results tables and in the data of Appendix A.

Table 1. Identification of Charcoal Samples

SampleIdentification

Date

Received

IML-I #5

IML-1 #1 3/1/93

IML-1 #2 3/1/93

IML-1 #3 3/1/93

IML-1 #4 3/1/93

3/1/93

USML-1 #1

USML-1 #2

USML-1 #3

4/15/93

4/15/93

4/15/93

2% Platinnm

Acid Washed

ActivatedCarbon

Activamd Carbon

ActivatedCarbon

2% Platimlm

Acid Washed

Activated Carbon

USML-I #4 4115/93 ActivatedCarbon

USML-I #5 4115/93 ActivatedCarbon

SLI-1 #I 515194 2% Plafinmn

SLI-1 #2 515194

SI.J-I#3 515194

SLI-1 #4 5/5194

SI.J-1 #5 515194

SLD-2 #1 515194

SLD-2 #2 5/5/94

SLD-2 #3 5/5/94

SLD-2 #4 5/5/94

SLD-2 #5 5/5/94

Acid Washed

Activated Carbon

ActivatedCarbon

ActivatedCarbon

2% Platinum

Ac_Washed

ActivatedCarbon

Activated Carbon

Activated Carbon

Estimated Total

Weight, g.

213

1523

285

499

493

348

1767

453

453

453

362

1750

506

503

501

396

1826

456

472

453

PI-STS-58 (SLS-432) 515/94 2% Platinum 114

P2-STS-58 5/5/94 2% Platilmm 113

.I

im

,.,. .

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' i i i i

SampleIdentification

Date

Received

ACT4-STS-58

Presumed

Charcoal Type

P3-STS-58 5/5/94 2% Platinum

AW1-STS-58 5/5/94 Acid Washed

AW2-STS-58 5/5/94 Acid Washed, |

AW3-STS-58 5/5/94 Acid Washedi

ACT1-STS-58 5/5/94 Activated Carbon

ACT2-STS-58 5/5/94 Activated Carbon

ACT3-STS-58 5/5/94 Activated Carboni ,

5/5/94

5/5/94

Activated Carbon

Activated CarbonACT5-STS-58

¸Estimated Total

weight, g.

113

714

716

717i

605

612

612

614

612, i

The analysis method used for these samples was thermal desorption coupled on line to

a gas chromatograph/mass spectrometer system. The specific instnmaentation and operating

conditions are summarized in Table 2. Unlike previous analyses, a dry purge was not

conducted prior to thermal desorption, nor was a Nation in-line dryer used to remove water

vapor desorbed from the charcoal. The impact of water vapor on the analysis was significant

but was minimirext to the extent possible by reducing the quantity of sample actually

analyzed.

To improve quantitative accuracy, standard mixtures were prepared containing known

concentrations of selected compounds that were among the most abundant in previous

scrubber charcoal analyses including those conducted at Battelle. This standard mixture was

analyzed for purposes of calibration by direct splitless injection into the GCflVIS system or

for purposes of estimating recovery by spiking onto a charcoal sample followed by thermal

desorption GC/lVIS. Initial trials using solvent based spikes onto previously desorbed

charcoal samples were not successful because the solvent created excessive peak broadening

rendering identification and quantification difficult. To overcome this problem, a pressurized

gas standard was prepared whose composition is shown in Table 3. This gas standard was

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used both for direct injection to single point calibrate the GC/MS system, and for loading

previously desorbed "blank" charcoal samples for purpose of estimating recovery.

Table 2. Instrmnentation and Analysis Parameters

: Charceal Analyms

Thernud Desorber:

Dry Purge:

Desorb Temperature:Desorb Flow:

Desorb Time:

GC/MS System:GC Column:

Initial Temperature:Temprann_ Program:

IoniT_tion:

MS Scan Range:

Scientific Instrument Services Short Path Thermal Desorber, Model TD-2

None

300_C5 mL/min

3min

Finnigan Model 4500

Restek RTX-5, 60 m x 0.32 mm ID, 0.51an film thic_ess-20"C, 6 rain

-20°C to 20_C, 50_C/min20_C to 300_C, 10_C/min

EI, 70eV @ 0.35 ma

29 to 300 Da, 1.0 sec per cycle

wat_ Aaaty_ frrimethytmine)

Insmm3ent:

Sample Introduction:Mobile Phase:

LC/MS Interface:

Ionization:

Operating Mode:Parent Ion:

Daughter Ions:Dwell Time:

Collision Energy CEt._):

Target Thickness:

PE-Sciex API m Tandem Mass Spectrometer

500 _L, How Injection (No Chromatographic Column)Water, 1.2 mL/min

Direct Vaporization (Battelle Vaporjet, 180°C)

Corona Discharge, 3 ma, APCI

Selected Ion ReactionMonitoring

m/z 60 (Protonated Molecular Ion)m/z 44, m/z 45658 msec

25eV

Argon, 350 x 1012 cm "2

4

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Table 3. Composition of Standards Gas Cylinder

Compound

Ethanol

Isopropanol,

Acetone

Concentration

ng/mL

30

30

30

2-Ethoxyethyl acetate I0

Benzene 10

Toluene I0

o-Xylene

Cyclohexane

Dibromochloromethane

Trichlorofluoromethane (Freon 11)

1,1,2-Trichloro- 1,2,2-u'ifluoro methane

(Fmon 113)

I0

I0

I0

I0

10

1,1,1-Trichloroethane 10

Butanol 10

Water Samples

Trimethylamine (TMA) analyses were conducted by direct aqueous flow injection

combined with tandem mass spectrometry. No sample preparation was necessary. The

instrument and configuration are summariz_ in Table 2. The tandem mass spectrometer is a

PE-Sciex API III configured with a corona discharge atmospheric pressure chemical

ionization (APCI) ion source and a proprietary Battelle interface which vaporizes the flow

injected carrier (mobile phase) prior to its entry into the APCI ion source. Water vapor

serves as the predominant reagent gas resulting in protonation of TMA (m/z 60). Ions of

5

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this mass are isolated by the first mass analyzer and subjvct_l to collisional activate_l

dissociation (CAD) using argon as a low pressure inert target. Two characteristic daughter

ions (fragment ions) are monitored for TMA (m/z 44, 45). The ratio of the daughter ions

serves as a highly selective qualitative feature while the daughter ion response serves as a

means for quantification.

Results and Discussion

Ci_rcoal Samples

Initial testing was coacerned with quantifying our ability to recover the standard

compounds in the cylinder gas standard from the charcoal samples. One sample representing

each type of charcoal was thermally desorbed for 20 rain., allowed to cool, then spiked with

I00 mL (measured electromcally as standard cm 3) then analyzed under the conditions

anticipated for sample analysis. A backup trap was attached to the exit of the "sample" to

detect any breakthrough of aualytes from the carbon sample. No target aualytes were found

in any of the backup traps. Results from these analyses of the spiked charcoal samples are

in Table 4. Percent recovery for each analyte was based upon the total ion

current in the background subtracted mass spectrum for the spiked charcoal sample divided

by an equivalent total ion current value obtained by direct injection into the GC of the

cylinder gas standard. Low recovery was evident in some cases. As an example, ethanol

and isopropanol were poorly recovered from the untreated and platinum charcoal samples.

These results suggest that longer desorption times may be a factor to more efficiently recover

these compounds, however on separate u'ials with unconditioned samples we observed that

longer desorption times comributed to degradation of chromatographic resolution presumably

as a result of additional water introduc_ to the GC column.

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Table 4. Recovery of Standards Spiked onto Different Charcoal Types'

Compound

Ethanol

Isopropanol

Acetone

2-Ethoxyethyl acetate

Benzene +

Cyclohexane 2

Toluene

o-Xylem

Dibromochloromethan

e

Trichlorofluoromethan

e (Freon 11)

1,1,2-Trichloro-l,2,2-

trifluoromethane

(Freon 113)

1, I, 1-Trichloroethane

SpikeLoading,

micrograms

Butanol

% Recovery

SLD2 #5

(Untreated)

% RecoveryUSML1 #2

(Acid Washed)

% RecoveryUSML1 #1

(Platinum)

3.0 3.3 19.0 2.4

3.0 4.7 18.2 5.9

3.0 12.4 37.8 35.0

1.0 6.6 67.2 55.8

1.0 25.3 54.2 52.5

1.0 31.5 47.6 33.1

1.0 27.6 35.9 45.2

1.0 2.5 30.7 15.2

1.0

1.0

16.8

21.2

15.8

33.4

1.0

43.6

53.7

51.9

28.1

1. See text for details.

14.6

26.1

27.6

73.8

2. Benzene and Cyclohexane were not chromatographically resolved under the

conditions of analysis in either the spiked charcoal samples or the standard from which

recovery is based.

o

A

Gravimetric results for each of the charcoal samples analyzed are mmmmrized in Table

5. included in Table 5 are the original weight of sample desorbed, as well as percent weight

loss presumably due to water vapor. Except for IML and USML charcoal samples, all

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samples within a mission set show comparable water coment with a slight positive bias in the

acid washed and platinum load_ charcoals. This u'end is not observed in the older IML and

USML samples which, despite precautions for maintaining a hezmefic seal, may have gained

or lost water during storage. The two "Blank" samples shown in Table 5 were each aliquots

of a single laboratory charcoal sample stored with IML and USML samples. The relatively

low water contentof thischarcoal combined with good agreement inthese replicateanalyses

indicatethatthe water contem of the samples issubstantialand thatthesemeasurements are

reproducible.

Table 5. Weight of Sample Analyzed and Estimated Percent Water.

SampleIdeatification

WeightDesorbed, g.

WeightLess, g.

WaghtLoss, Percent 1

IML-I #I 0.1432 0.0254 17.7

IML-I #2 O.1063 0.0197 18.5

IML-I #3 0.1133 0.0494 41.4

IML-I #4 0.1158 0.0097 8.4

IML-1 #5 0.1611 0.09.54 59.2

USMI,-1 #1 0.1377

USML-1 #2 0.2263

USML-1 #3 0.1655

USML-1 #4

USML-1 #5

SLJ-1 #I

O.1769

0.1142

0.1219

O.1823

0.1357

0.1263

0.1171

0.1076

SLJ-1 #2

SI.J- 1 #3

0.0253i

0.0374

18.4i

16.5

0.0214 12.9

0.0154 8.7

0.0109 9.5

0.0236 19.4

0.0359 19.7

0.0152 I1.2

SLJ-1 #4

SLJ-1 #5

SLD-2 #I

0.0134

0.0132

0.0259

10.6ii ii

11.3

24.1

8

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SampleIdentification

WeightDesorbed, g.

WeightLoss, Percent 1

SLD-2 #2 0.1095 0.0244 22.3

SLD-2 #3 0.1003 0.0208 20.7

SLD-2 #4 0.1242 0.0282 22.7

SLD-2 #5 0.1154 0.0246 21.3

P1-STS-58 0.1194 0.0313 26.2

(SLS-02)

P2-STS-58 0.1426 0.0356 25.0

P3-STS-58 0.1694 0.0414 24.4

AW1-STS-58 0.1772 0.0402 22.7

AW2-STS-58 0.1509 0.0355 23.5

AW3-STS-58 0.1280 0.0277 21.6

ACT1-STS-58 0.1666 0.0375 22.5

ACT2-STS-58 0.1816 0.0421 23.2

ACT3-STS-58 0.1262 0.0303 24.0i

ACT4-STS-58 0.1112 0.0245 22.0

ACT5-STS-58 0.1037 0.0228 22.0

BLANK #1 0.1175 0.0100 9.4

BLANK #2 0.1058 0.0096 9.1

1 Measured weight loss is presumed to be almost entirely from adsorbed water.

Chromatographic and tabular results are provided in Appendix A for one of the Blank

charcoal analyses and the three spiked charcoal samples described above. Note that the data

in Appendix A is organized so that tabular and chromatographic data for the same sample are

on facing pages. Following these data are tabular and chromatographic results from one

analysis of each unspiked sample. All of the chromatographic data in Appendix A were

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acquired under the same thermal desorptionand chromatographic conditions.Additional

analyses,for example splitinjectionsfrom the charcoalto the chromatographic column, were

carriedout in some casesfor diagnosticpurposes to betterinmrpmt (qualitatively)

chromatographic or mass spectralresults.Sample analysisresultsprovided in Appendix A

are represented as the identifiedcompound, an RIC value corresponding to the totalion

current response,the measured concentrationfor thatcompound, and in those cases where

the identifiedcompound was one of those in our gas standard,a correctedconcentration.

The corrected concentration was calculated as the measured concentration divided by the

fractional recovery of that compound from the same type of charcoal.

Sample//5 contained the most compounds and highest conccnwations in both the IML

and USML sample sets. These results are consistent with their presumed most forward

location in the scrubber. A decrease is observed in the methylene chloride concentration

with decreasing sample number in both sample sets, consistent with expectation. The results

obtained from these analyses identify some of the same compounds but at approximately 10

fold lower concentration. Some of the compounds identified, for example acc_ne in USML

were not present in subsequent samples. Many of the compounds identified from re-

analyses of the IML and USML sample sets were previously identified in these samples, but

now at significantly lower concenn'ation. This difference may represent loss of analyte

because of sample age or may be the result of excess water co--introduc_ into the

chromatographic system.

Results from the SLD and SLI sample setsshow similartrendsinthatSample #5 was

in each case the most heavilyloaded with organiccompounds. The lowestconcentrations

were observed in the #1 samples however a declining trend in concentration from the first to

the last charcoal sample in the collection sequence is not clear. Some of the compounds, for

example methylene chloride in the SLD samples, show an erratic distribution that does not

appear to be correlated to their position in the scrubber. Methylene chloride may be an

artifact of sample recovery or storage prior to delivery at Battelle. This compound is not

present in Battelle's method blank charcoal that was stored with the samples. The high

10 r_

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concentration of isopropanol in SLJ-1 #5 may be a contamination artifact became it would be

expected to be present in succeeding samples of that set. The STS-58 samples revealed high

concentrations of organic compounds in the activated charcoal (AC5 through AC 1) with an

apparent maximum concentration in AC3. As expected, lesser concentrations were observed

in the acid washed charcoalsamples (AW3 through AWl) and even lower concentrationsin

the Platinum loaded charcoals(P3 through P1).

Water Samples

Figure 1 providesthe actualsignalresponse obtainedfor each of the reaction

monitoring channels (60/44 and 60/45) resultingfrom flow injectionof a water blank, a 75

ng/mL standard,a 149 ng/mL standardand two injectionsof a 372 ng/mL standard. Both

channels arc recorded nearlysimultaneouslyby alternatingacquisitionof the two specific

daughter ions of TMA. The key elements of the TMA signatureare the presence of the two

daughter ions and the near equivalence of their relative abundance. The Ion transition at the

m/z 44 daughter ion (60/44)was used for quantification.The resultingTMA calibration

curve isshown in Table 2. Resultsobtained from analysisof the threeECLSS water

samples are sunmmrized in Table 6. Our limitof detectionfor thiscompound in water is75

ng/mL, and issupported by a calibrationstandardwhose resultsare distinguishablefrom

zero. Included in Table 6 are preliminaryresultsfrom electrosprayionizationtrialsthat

provided unconfirmed evidence of sodium cationand iodideanion in selectedsamples. One

of the samples containedTMA atthe limitof detectionwhile another was approximately

threetimes thisconcentration.The thirdsample provided a suggestiverespomc but was

below thatof our lowest standardand isthereforenot detected. Graphical resultsfrom

analysesof these samples arc shown inFigures 3 through 5. In each case,three injections

were made corresponding to a water blank, the ECLSS sample dilutedby a factorof 5, and

finallythe undilutedECLSS sample. Injectionof the dilutedsample was a precaution to

avoid potentiallyoverloadingthe ion source. In allbut the non-detectcase,WRT-STg--0108-

0-CETA-127-T-MFS, a clearresponse isobserved for TMA thatisgreaterthan the water

11

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blank or the dilu_d sample, and with a daughwr ion abundance ratio consistent with that

from the calibration standards.

Table 6. Trimethylamine Analysis Results for Water Samples a

Sample

WRT-ST9-O108-0-CETA-127-T-lVIFS

Trimethylamine

ng/mL (ppb)

¸:Sodium

¸Cation

WRT-ST9-0107-1-CETA-127-T-MFS 75 +

WRT-ST9-0106-O-CETA-127-T-MFS 240 + + + +

nd ++++

• Iodide

Anion

nd

X

XX

1. Samples were approximately 125 mL each, received on December 15, 1994

nd= not detected.

+ denotes incidental non-quantified observation of sodium cation, number of symbols

approximately proportional to response.

X denotes incidental nowquantifi_ observation of iodide anion, number of symbols

approximamly proportional to response.

In addition to flow injection MS/MS analyses for TMA, positive and negative ion

electrospray mass _ were acquired for each water sample. These results are shown in

Figures 6 through 8 which correspond to the background corrected mass spectra from flow

injection. An aliquot of each sample was diluted with an equal volume of methanol to

reduce surface tension and improve the stability of the electrospray process. Each figure

contains the positive ion and negative ion mass spectra for one sample. The spectra contain

evidence of coincident corona discharge APCI ionization in addition to electrospray

ionization resulting in several mass peaks due to protonated water and methanol clusters and

other unidentified species. Because these samples were described as having unexpected

conductivity, we have highlighted the presence of sodium cation at m/z 23 in the positive ion

12

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spectraand iodidecationat m/z 127in the negativeion spectrafor two of the threewater

samples.

Conclusions and Recommendations

The results obtained from the charcoal analyses represent a range of compounds and in

some cases unusually high concentrations of polar compounds such as ethanol and acetone.

The use of GC/MS to analyze a range of compounds is widely utilized for environmental

analyses, however this approach becomes complicated for charcoal analyses because of the

unusually high water loading. The older IML and USML charcoal samples did not show

consistent water loading nor did these samples reveal the same concentration of non-polar

compounds as determined under the previous contract. The remaining three sample sets

showed a variety of polar and non-polar organic compounds.

Analysis of the water samples for TMA was accomplished using flow injection APCI

tandem mass spectrometry. A detection limit of 75 ng/mL was obtained which allowed

detection of TMA in two of the three samples provided by ION Electronics. In addition to

TMA results, positive and negative ion electrospray mass spectra revealed qualitative

evidence for low concentrations of sodium cation (m/z 23) and, unexpectedly, iodide anion

(m/z 127) in two of the three samples. If absolute quantitative information for sodium

and/or iodide is desired, we recommend atomic emission (Na) and ion chromatography (1) as

the analysis methods of choice. These analyses can be conducted at Battelle using remaining

quantifies of these samples.

13

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Page 20: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

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L.

_DI

2.6

%

Page 21: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

I

lid 0 ID

w (-i_ "lul_ot:lIn

17

Page 22: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

18

Page 23: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

WRT-ST9-0107-1-CETA- 127-T-MFS

1LED5/Scan 25-fProfile Q1 SCANScans 25-25 minus 19-19 & 29-29 Time=-2.28 min1LED5 - 1/9/95 - 9:28 AM

NASA

1 peak 210,500

¢/)

19

t-I

19._>_¢(9n-

100-

75-

50-

25-

_>3.0

II

w

100

(a)

L__.._L.. t, ........... _ ..........

200 300

rrdz

1LED5/Scan 53-Profile Q1SCANScans 53-53 minus 4747 & 62-62 Time=5.07 min1LED5 - 1/9/95 - 9:28 AMNASA

175,000

o_

._z,t.-I9

t-

19

19n-

100-

75-

50-

100 200 300

m/z

Figure 6. Figure 6. Positive ion (a) and negative ion (b) eleetrospray mass spectrafrom WRT-ST9-0107-1-CETA-127-T-MFS.

19

Page 24: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

i

Page 25: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Appendix A

Results from Charcoal

Analyses

Page 26: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal
Page 27: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

.'lm.O

11/I?,'94 11tZ2Hk3 CW.Ix _I(_L. _ CUT OF" 290 _5_W_I,.IEn!11'__ _ SPL.ZTLESS2 llTN t 358CONDS.n6g1'1X L"ne_'1'1'110_R,I'II:'ILI'I _ _ Z5NANG_ G I. 1 LABEL: H O. 4.0 0_4_ _ O, 1.0J 0 IM_.t U20o 3

" I

!

ll.O

!

5:W

TOT_. DATA: Ig5,183 el 5CN,5 llOe TO _88e11/17_J4 II:12xSB C_,.1: 155401C_. _ ctYr IF _ TO 280__8 !14! _ _ _ 2 lqlH It 358 228_C134D5.t ill X L32 I,g'l l._li'i FIL.IM_ _ ISRNiCE2 C 1, 1 L,4B_t _ 8, 4.0 Ot,t_ _ e., 1.oJ o B_,.t u26, 3

5L2B.

_lnv _e_flV

29188

1311e 14_ 1380J l_lOJ 17_8_ 1808 15_ S_:_V,In

Page 28: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Peak No.

Gas Standard 198706

Identification

EthanolTrichlorofluoromethaneAcotolle

iPA

1,1_2-Trichloro-l,2T2-trifluoroethaneltlrl-TrichloroethaneButanolBenzeneJCyciohe_neToluene

(I mL injected)

RIC Value

351784160

28438467489922256

2297664256

Known

Conc (;m/mL)

0.0300.0100.0300.0300.0100.0100.0100.020

9 55360 0.01010 Dibromochloromethane 19488 0.01011 21920 0.010L2..Ethoxyethylacetate

rO.,Xylene 4659212 0.010

Page 29: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

I_TN. I_TA: _ el g_HS 280 1'0 flu

.gNP..£: 31 ft. _S S'm 2_C_145.e liB,t X S.3:2 I_ 1.5t_ _ ItlXS ES_ ISImlGEs C 1, I J,M£].J K 8o 4..0 _UAI_:R O, L.8 J 0 BASE: U 26, 3

-LN.8 ....

'OTRL.

"S7

400 G0e 790 806,SeW glq 0128 1Ol0O 1tt40 13"-29

7UT_L 0_TA: lN71JE tl _ 1108 TO 10ee11Jw7'_ 11:44:00 c_t.)t L,qS_ICAL. (J_ OUTOF" 200 TO lOO05N'PL_ _1PL _ _ 2200UC_HBS.: 685 X J.32 Pin l.St/5 FIU5 AT_ IESC lSI_ICF.: C %, z _OB.: I_ O, 4.0 GL,W_ A 8. 1.0. J O ik_ _26, 3

108.0

IS: lieleee1_:4o

10

12

11

• I

12N 1 1400 1500 1 I;5)6 188021_40 2_:28 2_toe 2_44) 28:20 _too

4_- 3co

Title

Page 30: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Platinum Charcoal 19900: 100mL Standa _1

Peak No. Identification RIC Value pg in 100 mL Measured

2

4

EthanolTrichlorofluoromethaneAcetoneIPA

1,1,2-Trichioro-l,2,2-trifiuoroethane1,1,1-TrichloroethaneButanol

Benzene/CydohexaneToluene

1888048832

44134485248

18508831O4O

29,5424219135O

3.0001.0003.0003.0001.0001.0001.0002.OOO

Amoum _g)

0.0730.1461.0510.1750.2610.2760.7380.52S

9 775168 1.000 0.33110 Dibromochloromethane 118400 1.000 0.15211 488448 1.000 0.55812

2-EthoxyethylacetateiO-Xylene 1.0001017850 0.4S2

Page 31: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

TUT_K. _TA: _ 81 _ 2m TO 210811/18/54 14:2_80 _f.I: 15mSl_L 0G CUT (_" 282 TOSNg_.£: 18e PL _ _ _ TO LSPt.OI-I 2 _ _

Ca41_t SN5 X 8.32 J_ 1.5LI5 nL.q I_IX5 ESC IS

C 1, t t.Mfl.: H Bo 4.8 0t/_: A O_ 1.8 J 0 iJASEs U28, 3

488.0 ....

rOT_.

4 6

, • • i . •300 400 500 600 7'005JOe (;:q 8s28 18:88 11:40 13-2B 15:M

]

I 10

|

18L0

TOTAL I_TR: 159113 el _ llle TO lale

11/18/94 14:31G:m CALl: 1_I_IC_ fIG OUT OF 2m TO lNB_n IN I'lLG_ _ fL_M.]_ TO U_OI-I 2 HINI_ _l'l_

OONDS.s ImM X L22 _i I.RJI_ F'II.I_IrrX5 DES_ IS

I_(G[s G 1, 1 L._El.n H O,, 4.0 OLIn: A 6, 1.0 J II ORSE: U2O, 3

2342518,

12

11

I

21b:_

i13M

21:4_

I ' I I I J14_ 1588 ISM I788 18M

45- m

TItlE

Page 32: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Pe__kNo.

Acid Washed Charcoal 199C

identification

Ethanol

06 10OraL Start, lard

RIC Value

147968

IJg in 100 mL

3.000

MeasuredAmount (pg)

O.57O

2 Trichlorofluoromethane 145408 1.000 0.4363 Acetone 476160 3.000 1.1 344 IPA 266240 3.000 0.547567

10

37990458304

1125122260990

1,1,2-Trichloro-l,2,2-trifluoroethane1,1,1-TrichloroethaneB,___anol

1.0001.0001.0002.OOO1.000

Benzene/Cy_ohexaneToluene 1116150

Dibromochloromethane 238848 1.0002-Ethoxyethylacetate 5811_r6 1.000O-×ylene 807936 1.000

1112

0.5370.5190.2810.5420.4770.3070.6720.359

Page 33: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

.4N.0

rTN.

101"N,. IDPJAs_ el SC1_5 _ 1_0 lira11_0,,_4 18a21em CI_x l.qESBICIL eG _ f 200 TO 2000

IN IL GnS STD e/'Pl.l_ T0 UgLel-2 _'IINI_5_ Sic'I-I1LE_COHI]S.s BIll X L:I2 II'l 1.SUI_FILII Irr_ IIE3C ;S

G 1, I _ H O, 4.11 _ll_s _ |, &.eJ 0 BASEs U21, 3

2

m a " ,,,,' ' ,,,' ' m5sin 614e 08m |Ibm Ilnq 1313

IO0.O

TOtaL I_ITAs LqSM6 II1 5C1_5 lille TOII/10.AJ4 16s2MIm CALl: 1_qQSBICAL.N OUT(F 200 TO 2He._I_I.E, IM It. GI_ 511) IPPLI'_ TOUSl_el-2 2Mll3mC Slq.21UESSt_l_S., _ x 0.32 R,e1.5.11 FILIt RT_ I]ESC 15

C 1, 1 iJIBEIJ H $, 4.0 _ A 0, 1.0 J e _ U29,, 3

Jt_16e4e

I

26318'/8.

r' '

12

11

• ! !

131m21s88 21s48

L _ .. A _ nn

' I ' / i J I !

14/8 1_ 1600 17'ee IN8 l_le23:2B 25:00 26_4e 2B_2_ 30:00 31:40

4,.',- m

l

TIRE

Page 34: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

; lOOmL Stanclard

Peak No.

1 Ethanol

345678

Untreated Charcoal 19890,

Identification

1112

TrichlorofluoromethaneAcetoneIPA

1,1,2-Trichloro-l,2_-tdfluoroethane1,1,1-TrichloroethaneFButanol

IBenzene/CyclohexaneToluene

RIC Value

81552

pg in 100 mL M___$umdAmount (pg)

3.000 0.09886400 1.0001 0.168

262656 3.000 0.371134400 3.000 0.141

1.000 0.2121.000 0.158

2304O026240

2035710 2.0009 1019900,

10 Dibromochlommethane 245441415682-Ethoxyethylacetate

O-Xylene 832512

0___¢31.000 0.3151.000 O.a=£1.000 0.0661.000 0.276

Page 35: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

'40O.8

TOTW. mT_ _ el _ 200 TO 110011,419,'$4 18diSsm CAL.It _I, CPd.II15 OUT _" 288 TO _B08.S_qPUE_lm eL G_S STD N_L.ZED TO CH_COAI. 2 lCZN! _lmC SR.TTi.[_COI4DS.IGiel X 11.32 N'L 1._1,1 FII.I'I liL'TXSOES_ ZSIMHGEs G J,, 1 _ 14 O, 4.8 _ A 8, _..ll,n S _ U28, 3

23 G7

5808 6s40 0_20 lOxm 1LI4O 13,t28 15: 00

100.0

TOTN.. mTAs 2_ OI _ 1108 TO _0011,,5B,94 18tlJ_llO CIL.iJ 1.q8581ClL OZ5 OUT OF 200 TO 2000

108 15. GASSllD W_Yl_ TO CI4N_C_L.2 MlNt 3_0C SPL._C_HOS,z SUMX 0,32 lgl I._UH FZJ..M_ ESC ISliU_N_z C 1, 1 _ N Q, 4.8 81.1_x A II, 1.D,I 8 BA_s U 28, 3

l

10o815:4o

II°' I

1804tSL

12

11

J

12ee2o_o0

I " / " I i 1

i380 1400 1500 1600 17'00]

LO0030800

Lqo03Ls44_

4S- 300

!

Page 36: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

IML-1 #1 Compoundl Identit'md

Methylene chlorida

Peak No. Identification RIC Value

1 Bromotrifiuoromethane 358402 3672

Conc (,._,njg) Conc (,.+,miD)Meres. Corr.

0.621 b0.064 b

a Quantitation based on an actual standard compound.b Quantitation based on comparison to average of three haloj_ermt_d stand:_.rd compounds.c Quantitation based on comparison to average of four non-halogena_d standard compounds

Page 37: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

88.0

rOTN.

110TAL DATA: 1518m4 01I1_113_4 J4tl4Jm t:ALIs Im381CJ:K. e55Ng'_n IL-IO_ SI'LI'ILESS 2HTNt 3t8C 1?80Vt]X4t_.: inn x 0.32 _ L._ln FZL..tK'TX50ESG I5le_G£a ;

5:00 6:10

2001'01108Ct,'TOF 288191800

1, ! _ 14 O, 4.0 _ A |, 1.8J e _ U3J, 3

2

i i i i i l !

588 Elm ;50 880 _ 10000:20 lliaO0 tk:40 1_6 15,08 lGt4e

TOTJtL [h_T_ 15i8m4 01 _ 11.88 TO 180011_/4J4 14:14t00 CALls 1_q838]CI_L41_ OUTCF 200 TO |oOesw,Pt.l[: I/L-101 _ 21,11Ht35B: 171t.JCa,iflS, t ElMX L32 Ig'l l.gJPI FIL.H RI"_ OESCI5RN4_.t G 1, 1 UiEL: N 8, 4.0 0O_: A 8, 1.0 J O _ U28, 3

108.8 51m.

45-3100

1200 I_ 1_ 1500 1_8 175_ INO20:8e 21:4e 23:20 25:00 2S:4e 28 20 3e:ll

S_mTIHE

Page 38: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

IML-1 #2 Compoun"

Peak No.. Identification

1 Bromotrifluoromethane2 Dichlorodifluoromethane345

1,1_-Tdchloro-l,2,2-CrifluoroethaneMethylene chlorideAcetic acid

1,1,1-TdchloroethaneBenzene + CyclohexaneToluene

; Identifmd

RIC Value Conc (ug/g) Conc (ua/g)Meas. Corr.

22720 0.530 b3600 0.0841 b5064 0.076 0.141 a

95616 2.231 b85408 0.279 c4472 0.173 0.334 a2014 0.006 0.011 a2680 0.006 0.012 a

Caprolactam 12960 0.042 c

a Quantitation based on an actual standard compound.b Quantitation based on comparison to average of three halogenated standard compounds.c Quantitation based on comparison to average of four non-halogenated standard compounds.

Page 39: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

'40O.0

0TRL.

TOTAL. W_I'_ _ 0111,413._4 |3_u3_m C_LIx _ll_L (1_

ILL-102 _ _ _ 17WUCONDS.m6m'[ X ik_ I_ I.RII_ FIi.J'I Im_ IESC

I I i !

3100 400 glR_R 6:40 8:28 108m

_ T0 IIM0UTOF 2B0 T0 IB_

5

tl,46 13n20 I_R 16.40

TOT_ I_lTAz Lg_B3 el15/83,'94 I_3_N _LI: 1_301C_. 1'3

ZI'L-102 SPJ.Z'P..I_ 211IN__aC I_CIM_._ _ X 11.32 e_ 1.5U1_FI.I.Pl _ 0E_Itm4G_ G 1, 1 I..,_E_ N 6, 4.0 GUe_ A |, L.0,J 8 BRSE, U20, 3

I08.0

,¢5- 3ee

9

i I | I I I _ I

TIME

Page 40: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

IML-1 #3 Compounds identified

Peak No. identification RIC Value Conc (pglg) Conc (pg/g)Meas. Corr.

BromoU_uoromethane

2 Methylene chloride3 BP 45, 61(50)4 ep 31, 45(85). 61(50)5 Xylene or Ethylbenzene6 Phenol7 L.Jmonene 3508

14640 0.35170784 1.697

200192 1.01815104 4.1326163O28

8 Benzoic acid, methyl ester, 42569 Methenamine 208128

10 Caproiactam 8992

bbC

C

0.013 c0.015 c0.018 c0.022 c1.053 c0.046 !c

a Quantitation based on an actual standard compound. IIb Quantitation based on comparison to average of three halogenated standard compounds. Ic Quantitation based on comparison to average of four non-halogenated standard compounds.

Page 41: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

:388 _ _ _ _ i _ IBN_W 6:48 On_ l_m llJ_ 1_ I5:m IGz_

COHOS.: _ X L32 I_ 1.SJn FLI.N RTXS 9ES_ ZSI_Vi_: r. 1, 1 _ H O, 4,0 OJmu A O, 1.8,J 0 BRSEI U2S, 3

3793S_

,45- me

Page 42: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

PukNq.

IML-1 #4 Compound

45

10111213

Iden',ification

1 Bromotrifluoromethane2 DichiorodWuorontethane3 2.Propenal

Methylene chlorideBenzene + CycJohexaneAcetic acidToluene

Xylene or Ethyibenzene2-ButoxyethanolTrimethylbanzeneLimoneneMethenamineHydrocarbon

s Identified

RIC Value

274432854415456

5171203996

18O8O

Conc (polo)Meas.

6.4370.2OO0.077

12.129

Conc (PD/O)Corr.

0.017 0.0680.090

3148 0.011 0.0351846 0.0002872 0.0141638 0,0086944 0.03417152 0.085428O 0.021

bb

!ciba

a Quantitation based on an actual standard, compound.b Quantitation based on comparison to average of three halogenated standard compound_sc Quantitation based on comparison to average of four non-haloger___ted standard c_.nml)ounds.

C

a

C

clC

C

C

C

Page 43: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

-flm.o

IR.e

_TA: Im409 OlTOTA[.1B/'2_ 14:21:M.T,BJ_I.£n II9..-I_, SP_._ 2 HI# DES_N JMC 17f0_KE.n 68'1X L32 em 1.SLm F1L._ K'T_ DESC I5l_i_i_.: G 1, I i..a_s H O, 4.8 _ A i, l.OJ O _ U2B,

4

lls4_D

SC_t5 _ "PO11MOOTCF ZM?O_

2 3

, _ _ "L..-- , J_ . - , S6_,3m ,lee _ 61m Bm5:M 6:411 k28 lkm I_

TOTfL DRTA: Lq04119O1 _ I|U TO1_ 14822rm CALl: Lq8301CAt.41_ lOUT_ 215 TO

CXZ_6.a 68'1X $.32 m l._t.l'l FIU'I Iff_ 9ESC ISI_e_E: G 1, I I._SEL: N O, 4.0 GU_i_ _l O, 1.0.J e ill, E: U2_. 3

!

16:48

7q i

,147,188.

8 9 10 11 1_L_3

, _ ' I ' ,'' Ii " I _ I- " ' I12Se 1_ 14m ISle 1600 1;'8828:0e 21=48 23-28 25:_ 2st4e 28=28

I 1 "' ' I

3e:Oe 31:48 TIME

Page 44: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Peak No.

234667891011121314

IML-1 #5 Compound

Identification

Bromotrifluoromethane!l_-Dichioro-l,l._2-tetrafluoroethane!Trich!orofluoromethane

s Identit'md

RIC Value

12544043776

226816

IMethylene chloride 512000Iisopropyl alcohol 246784

301568IBP 31, 60(50)IBP 3t, 61(60)

Toluene

Xylene or EthylbenzenePhenolBenzoic acid, methyl esterMethenamineCaprolactam

2.1150.7384.3088.632

19.2451.073

91264 0.32528960

a Q_,J___on based on an actual standard compound.

9776607226887912

3302404636

0.0890.0250.0220.0100.0281.1750.018

Conc (IJglg)Corr.

b Quantilation _l_,_¢edon comparison to average of three halogenated standard compounds.C

25.614 a

410.332 a

0.352 a0.078 a

C

C

Quantitation based on comparison to average of four non-halogenated standard compounds.

Page 45: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

TOTf_.. DATA: 1504410tli16,'24,"54 13:_Stlle IN.I: ZS83eIC_L 05Se_PI.E: ]et.-t05 SPLI_ZS5 2 I_lH e 350C 1711_CI]4DS.: Sll_ X '_.32 lgl I.:U_ Flt,,N llr_ ESC L_RN4GE_G 1, I _ I,I O, 4.8 a.i_ _ O, 1.0 J

408.0 - -- •

rOTl_.

1 2

300 4O05sO0 £:4e 8=3

180.0

208 TO 11N0UTIF 20e T0 200e

li_F_ U 21,, 3

4

6 7

I " ' '

700 _ 900IOsM llt'M) 13s28 lSsllO

TOTN. DATk: 150441e 01 _ 1100 TO 208818,,'24,,94 13z:_:OO CNL..IzL583OICW.. tS 0L_ I_ 200 TO 2080SN_L._t lJS.-le5 _ 2 HIH It 350C ITIJOUCOHDS.: GJl5X 0.32 191 1._u_ FIUq _ WSC ISRI_4GEsG 1, 1 LABE_ K 8, 4.0 GUN4x A 8, 1.0 J il Jq_: U28, 3

9

I *

l Jill16_4_

I

_q,.m12.

45- 388

13

TIIqE

Page 46: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Peak No.

4

5

6

USML-1 #1 Compound:

identification

Bromotrifluoromethane

Dichlorodifluoromethane

Benzene

Toluene

Xylene or Ethylbenzene

Phenol + Benzaldehyde!Hydrocarbon

a Quantitation based on an actual standard compound,

; Idantit'md

RIC Value

31968

6984

31761492

1144

1834

1092

Conc (pg/g)Me_s.

0.4520.099

0.007

0.002

O.O02

0.003

0.002

Conc (l_g/g)Corr.

0.014

0.006

b

b

s

a

c

cc

b Quantitabon based on comparison to average of three halogenated standard compounds.

c Quantitation based on comparison to average of four non-halogenated standard compounds.

Page 47: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

0K.I)

rYAt.

TOTN. DATAt _ 01 _ 280 TO ltm1147,,54 13tl?elli CI_I..1oI.q8301CN. 8_ GUTO_ 288 TO 2080.gqgs'l.EtLSI'L-1Ol SFLI'II.EE 2WWC0iCS. j 61fl X 8.32 im 1._15 FUJ_ IL'YX5IESC ._

G 1, I _ 14 4, 4.8 OUN41Ali, l.llJ I _n U28, 3

1

_m _o

3

8820 ShOO [le40 13s2O IStm IGta

"UUIW. IIi_T_ 1SB788 I)1 SCN45 1100 TO 2808ll,517,vS4 13;I'hli8 13M.Is ISB301CAL.I_ OUT OF 28e TO 2800Stoics.El WIS,-10I SlIS.FILESS 21UNtCI_S.# 68flX Ik32 HI _..SlR FJ[LI! IL'T_ DES_ IS

G l, I LME_ N El, 4.0 8Umb _ 8, l.eJ I illS[_ U2B, 3

Jm.8 154O8.

6 7

2_Oe 2"1t48 23:26 25:e0 25t4e 20,_9 30sO0 3_.s4e TL_

Page 48: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Peak No.

1

23

4

5

6

7

8

910

11

1213

1415

16

17

1810

20

21

22

Sulfur dioxide

Chloromethane

USML-1 #2 Compound..

Identification

HydroxyacaUddehyde1,1,2-Trichloro-1 _?.-tdfluo roethane

Methylene chlorideI-lexane

Trichloromethane

1,1,1-TrichioroethaneBenzeneAcetic acid

Toluene

Xylene or Ethylbenzene

2-Propenoic acid, butyl ester

StyreneBenzaldehydeHydrocarbon

TrimolhylbenzeneLJmonene

IHydrocarbon12-1=uranmethanol

Identif'md

RIC Value

132352

1776O

244736

88192

74368

1332837568

2371222496

382464

7848

2476

14288

1371214288

5472

338O

54965S20

7S68

Conc (i:g/g)

0.150

0.153

O.2770.433

0.640

0.015

0.323

O.4640.031

0.433

0.006

0.003

0.016

0.0160.016

0.006

0.004

0.006

0.0060.009

0.006iHydrocarboniNaphthalene

4952

3776 0.004i

Meas.Conc (pg/g)

Corr.

0.808

0.8950.057

0.013

23 Hydrocarbon 21824 0.028

24 Hydrocarbon 10080 0.011

28 Hydrocarbon 5648 0.006

a Quantitation based on an actual standard compound.

b QuanUtabon based on comparison to average of three halogenated standard compounds.

c QuantJtatJon based on comparison to average of four non-halogenated standard compounds.

cb

ca

b

c

b

a

a

ca

c

c

cc

!cic

c

cc

c

c

c

c

c

Page 49: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

,e

0ATA: _ el _ 206 TO Ill11/07,'9,1 t'_,31sO0 CaqL.]s_ICnL 415 OUT IF _ TO 2808Sef_vS..E./LISM.-II2 S_15.lTLJ[33_ _ 2288U_NOS.t Offt X L32 It't l._iJn F'ILFI RllQ leg: IS

_ I, 1 _ 14 iJ, 4°0 aUA04: _ Oo 1.0,J 8 EJ_Es U 2B, 3

4m.e - --

4

5

2 7

9

I 3 e

610 _le 8OOIAZ8 lOS08 llf4e |312e LStW

TOTAL gAl"m 1587_ el11_17_J4 12131100 CALII IS8301C_LgmPt._ W_-l12 SFLTrLESS25_Xt _OC 220_COHOS.: iSfl X 8,32 M l._lfl F',L.qRI'X5 DESCISIW4_: G 1, 1 I.WEL: t_ Io 4.80LIN_ R 8, 1.0 d

_n'GF _ "_ 21M

e BASEs U 20, 3

10

11

! I

IMBe

lOLl) 17'04_5.

45--30O

13 14 15

120e 1308 1400 l$lO 1560 17110 llllO 1911 Sl:;ltl21hllO 21:40 23:20 25see 2Gr4_ 28:2e 30see 31s46 TIME:

Page 50: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Peak No.

USML-1 #3 Compound:

identification

10

Bromotv_uoromethane

DichlorodifluoromethaneChioroethane

; Identified

PJC Value

91648114688

Conc (pglg)Meas.

1.3731.719

2920 0.044

4 Methylene chloride 202246 3.031i5 Acetic acid 0.0096 iBenzene

44481

20021992

4336

3144

3308

Toluene

2-ButoxyethanolSiloxane

Hydrocarbon

0.004

0.0030.009

0.007

0.007

Conc (pg/g)COIT.

bb

b

b

o.0151a

0.009 a

c

c

c

11 Hydrocarbon 4656 0.010 c12 Hydrocarbon 25088 0.053 c

13 Hydrocarbon 7056 0.015 c

a Quantitabon based on an actual standard compound.

b Quantitation based on comparison to average of three halogenated standard compounds.

c Quantitation based on comparison to average of four non-halogenated standard compounds.

Page 51: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

_OTAL

IO1W.. DRTAs 198597' 41 _ 290 11) Lirali_ ISs22sM CRL,I: 198301C_.. tl_ OUTOF _ I'U lMe_: tr:_l't.-143 5PI.,.I'11.,I_'_.2R.lal _ 17"ll0U¢1_S.: 68_ x 6._ I_ 1.51/_ F_iJ4 TI_ IE_ LSlilViGEiC 1, 1 i.llBEl.I 14 0,4.0 OI,W_ II ii, l..OJ 0 Ilia: Uit., 3

lie.l

TOTAL OATA; I_'? I! _ 1182 TO IBmII,,_.,'94 16;22:W CRI.I: 19_IOICRL I_ OUT OF _ TO I_

I.lSPL-IIi3 _..i'rt.E_ 2_HB _ IMClliD_: Iliel X li.32 lil l.Slll Fii.il RIX5 I)(SC iS_l C 1, l I._.s K 8, 4.0 QI.i_; R 8, 1.9 J @ Bl:i_l U _il,, 3

IMe15tq

1844_4.

i

_8

126_ 130e 141_ !

10 I_

_44_ 28:26 _:_ T]I"_

Page 52: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Peak No.

1

2

7

89

10

11

12

USML-1 #4 Compound:

_ Identification

BromotdfiuoromethaneiDichlorodifluoromethane

Methylene chlorideBenzene

Acetic acid

l-Hydroxy-2-propanone

2-Butoxysthanol

Phenol + BenzaidehydeHydrocarbon

TrimethylbenzeneI imonerle

Hydrocarbon

13 ;Hydrocarbon

14 iHydrocarbon

15 Hydrocarbon

Identified

RIC Value Conc (pglg)Meas.

128128 1.7SS

131071i

S37600

3008

1939227456

14272

3532

103048528

22304

10896

6336

1.830

7.537

0.005

0.038

O.OS40.028

0.007

0.020

0.0170.044i

0.021

0.012

20960 0.0415624 0.011

Conc (pg/g)Con.

0.022

a Quantitation based on an actual standard compound.

b

bb

;a

rcC

C

C

C

C

C

C

C

b Quantitation based on comparison to average of three halogenated standard compounds.

c Quantitation based on comparison to average of four non-haJogenated standard compounds.

Page 53: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

TOTN, f_TA: I_586 el11,4D,'_1%5:42XB CCL.i: 1.qSmICAL. 4_SRJSPLE:USIS,o]e4 5PI_ _5511.18_ 178_CCJ4DS.s Uel x 8.32 II't 1.SUM FIL.J.IRTX5 DES_RN4_t C 1, 2 _ N 8, 4.0 GI.J_ A 8, 1.8 J

00.8 ....

tOTAL.

12

_ TO 1188_ _TO_

B_ b 28, 3

3

388 4110 508 68e 780 8m58 0e 6t4e o:2e IO:.00 11:4e 13:20

188.6

TOTN. DATAs _ 411 SC/V6 1100 TO 1_11,,'0_,'54 15J42J00 C_.In 1JH381CIV,.115 OUT G_ 288 TO 180eSdV_LEm US_-104 SPLllU_S _ 350C 1711_CONCS.u SS.I X L32 N'J 1.SUII FU..15RT_ DESC LSRidGE: G 1, Z _ 0_ 6, 4.e ;u_: _ 8, _.0 J e _ u28, 3

4 5

I I

98815100

6

limIGs_

4094?2.

4_- 3IN

11 14

_89',o I, .... 1.3

20:.08 _:q 23t20 25:08 26:,_ 20J2g 30s0e TIIIE

Page 54: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Peak No.

1

2

3

4

USML-1 #5 Compound

Identification

BromoUifluoromethane

Chlorotrifluoromethane

Dichlorodifluoromethane

1,2-Dichloro-1,1 ,?,2-tetrafl uoroethane5 Dichiorodifluoroethene

6 Ethanol

7 Acetone

8 Trichiorofluoromethane9 Dichloroethene

10

11

12

1314

1516

18

19

Identified

RIC Value

32456

162816

Conc (pgig) Conc (pgYg)MeAs.

0.7053.536

Corr.

45696 0.992

21856 0.475

85504 1.857

4933430 52.762 1608.603

5029640 58.520 473.465

3784 0.098 0.58123584 0.512

1,1,2-Trichloro-l,2,2-trffluoroethane 1054710 14.706 69.239

Methylene chloride 1374462 29.8502-Butenal 13952 0.042Acetic acid 30358 0.092

69245 0.196 0.774178432 0.385 1.160

8528

320O1

1744O

5384

Benzene + CyclohexaneToluene

Xylene or Ethylbenzene

17 Styrene

Benzaldehycle

Methylphenoi (cresol)

0.026

0.0100.053

0.016

a QuantitaUon based on an actual standard compound.

b Quantitabon based on comparison to average of three halogenated standard compounds. !

b

b

b

a

cc

c

c

c

_c;8

c QuantJtation based on comparison to average of four non-halogenated standard compounds.

b

b

aa

a

b

a

b

Page 55: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

4eL0

rOTN,.

"JrOT_ 0AT_ IN505 el _ _ 10 lllmll,_t31_j4 I_02lW CN.18 L,q_OIr,,,_LI_ OUTOF 211 TO INI

IJSIL-le5 g'L_ 2 nZNll _OC 17110_C_IDS.: 611.1X L_ ell 1o_l.q FIU.i Irrx5 Wsc IS

G 1, 1 _ N 8, 4.0 GIW_ A 8,. 1.0J 0 _ U20, 3

11

10

2

3 4

5,m 6a,NI k20

11

7

S1

• .1 14

i;m _ 800 _elkm lls4e 13=20 I_N

I

limbIG:40

16

!

IN.0

TOTN.. OATI_ 150505 el _ IIM TO IWISII,43.,'g4 l'Jig2zm CALl: lS0311Ot _ OUT OF 201 i_ INtSNI%.E; USIt.-105 SR,ZTI.E_ 2 PIINII _OC 17eIJ(:Z_CS., aM x L32 m L.SJR I_JI prl_ I]£_ IS

G 1, I _ K O, 4.| Gu_. A o, 1.0 J 0 _ U_, 3_lra4.

4S- 3oe

|

18 lg16 17_ . _ , _ ,, ,.

1200 13ee 1400 1 1688 1710202ee 21z4e 23_20 2_ eo 26 4e 28:.20 30:08 TIME

Page 56: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Peak No_

SLD-2 #I Compounds

Identification

Identmed

RIC Value conc (l_o)Meas.

1 Sulfur hexafluoride 37120 0.762

2 Bromotrifluoromethane 14064 0.285

3 DichlorodifluorometJhane 5800 0.117

1,2.-Dichloro-l,l,2.,2-mtndluoroethane 10104 0.020

Conc (pglg)Con'.

5 Methylene chloride 77712 1.5746 Benzene 9t4 0.003 0.006

7 Acetic acid 1920 0.006

8 Siiane 3564 0.011;

9 2.Butoxyethanol 2948 0.009

10 Hydrocarbon 2280 0.007

11 Trimethylbenzene 1572 0.06512 Limonene 2652 0.006

rbrb

ib

!b

_b

:a

°Ic

c

opc

c

13 Hydrocarbon 1844 0.006 c

a Quantitation based on an actual standard compound.b Quantitation based on comparison to average of throe halogenated standard compounds.

c Quantitation based on comparison to average of three non-halogenated standard compounds.

Page 57: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

T0"iYL 6I_T_ _ elI0,,21,,g4 17a'_"LsN Cl_....In_ICIL

_LIO--2el S_..I_ 211INIE300C:I?'0OVC_l,10fks Hel X L.32 _ O.gUH FILJ'I_ S,_4 $4392IMHGEaG 1, 1 _ 14 O, 4.0 WAils A 8,. L.SJ

4N.8 - --.

'OTl.

2m TO llmOI_IF 2m TO 2Ore

2

I

G,,IO k20 10nJ

_U_ 3

8

'----"-I ; - I ; ] / I I r I

_sm 11|O _z_ lSsn IGI4Q

DATA: I_ II _ tin 1"01_ I?a_iN Cat.:: tJ8301_L I_ OUT OF" 200 TO 2800

SLD-2Ol _P_.._ 214I_1E3_0C:ITUUCOHC6..x 61i4 X 0.32 Pll LSUI_ _I..H _ .T_,"H_4,._52RAH_ G 1, I L.n_.s N 0,4.80U_s _ O, I.li,.I O IDlEs U2_ 3

1_8 7L2_E.

45.--3_

_ , _.9 1011 12 13

-_*_ _ -

20=M 21sq 23:_ 2_m _nq 2Bs '_m :3k_ 31s40 TI']NE

Page 58: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

P_kNo.-

SLD-2 #2 Compounds

Identification

identified

RIC Value Conc (IJg/g)Meas.

Conc (pa/g)Corr.

1 Bromotrifluoromethane 11t68 0.2222 Acetic acid 14496 0.045

3 J1,1,2-Trichloro-1 _,2-trifluoroethane 6056 0.077 0.143

4 Methylene chloride 356864 7.103r

5 Trichloromethane 1672 0.033847 0.0036 Trimethylbenzene

7 Unknown siioxane 7720 0.024

8 Caprolactam 2568 0.008

a Quantit_ion based on an actual standard compound.

b Quantitation based on comparison to average of three halogenated standard compounds. Ic Quantitation based on comparison to average of three non-halogenated standard compounds.

b

c

a

b

b

c

c

I

Page 59: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

9001.sag0

J

Im

TOTL _TAa 1.qo309#!tO,_lg4 l£:3osoe Cg_Lln_l_;al.

SU)-2e2 SPLITIJ_; 2PLY_ 27W uC04D5. a 6ael X e.32 M L=UH FILJ! _ S,,H _

G I, ! _ H e, 4.0 GUm _ O, 1.O,J

1lira 1o 21oo(£,.T _F 2N TO 2m_

34,,,_o

,,¢5- 3_

76

, [ .m _

I/:300 ' t- •14_0 't_lOO_,n,_ 21s4(I "_a3 2_tm

8

lltl |'/111 -' |ill I|

25x46 2O_'_a 31tffi 31s441 TTrlE

Page 60: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

SI.D-2 #3 Compounds Identified

Peak No._ I Identification RIC Value Conc (IJg/g)Meas.

Sulfur hexafluodde 1.36062592

Conc (IJoin)Corr.

J

2 Bromotrifluoromethane 22688 0.4933 Dichlorodifluoromethane 4744 0.1034 iTrichlorofiuoromethane 5240 0.126 0.7505 Methylene chloride 229888 4.9966 Benzene 971 0.003 0.014

ia Quantilafion based on an actual standard compound.b Quantitation based on comparison to average of three halogenated standard compounds.c

bbFa

_b;a

Quantitation based on comparison to average of three non-halogenated standard compounds.

Page 61: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

TOTIK. DRTAs 19831/ II10,'21,_J4 15t52sm CIK./: 158381CN. 155N'IP't.E: 9,.D-2l_ 5P1.I'13.£_ 2q_8_8C 1708/C_IDS.s mix 8.32 1t91t_Ul'l F'K.I'I A'IX5 .T_I4 5,1_2IWGF.I G

4418.1 ....

SC_H5 280 TO 1180D,,IT _" 2il6 T0 20e0

1,, 1 _ H 0, 4.0 0UN4t A 8, 1.8J S ONSEt U28, 3

5tin J.3_20

1

6s40 8t28

5

4

lkm 11t40

TOTAL DAT_. 158387' 0! 5_J45 1108 TO 218014b'21,,54 LSle_tm CALIt 158381C_L 15 OUT _F 288 TO 2888_SPf.E: KD-203 _ 2liDIt_SC 1708U

COHDS. i _el X L32 M L_lel FIt.lq lin'_ S,,N 54332G 1, 1 _ N 8, 4.e SUN4: n 0, 1.0 J 0 O_E.t U28, 3

180.8

$r"

i"588

15:08 16:48

_r

221440.

45- :38e

I ' I-- + " - l' " ' ' " I --'" | .... i l1208 1_10 14a 1N 1688 17N 1880

i I

31:40 TINE

Page 62: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Peak No_

12

SLD-2 #4 Corn oundl

identification

Sulfur hexafluorideB_uoromethane

, Identified

RIC Value

2368O18816

Me_s.

0.4160.330

3 Chlono4dfluoroethene 302080 5_014 1,1-Dichioro-t,l_4elTafluoroethane 3932 0.0695 2-Methyl-1 -propene 20192 0.055

Trichlorofluommethane

1,1._-Trichioro-l_.2-trifluoroetharueMethylene chlorideXylene or EthylbenzeneTrimethylbenzene4-Ethenyl-1 A-dimethylcycJohexeneHydrocarbonNonanalDecanalMethenemineHydrocarbon

67

1011

265607O55363988482108256832801330276O282453204576

1213141516

05t67.8906.9990.0060.0070.0090.0040.0080.0080.0140.01:

3.068_ac

37.1460a

a Quantitation based on an actual standard corn ound. []Quantitation based on comparison to average of three halogenated standard com__ _ o'n _ _ a--_"m-_ _ _ __e--"ed-'m-n_-'_ compounds.

Page 63: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

_lrL

7

8

I I I I i I I I

300 400 3110 cam _ aim 900 liilO5ira 5:q Olin llilm ll:q 13s20 1.58i I_n40

TOTAL O_TAs 199306 gl _ llm TOI0._I/_I _sllgsa l_l.l_ I_ICII.. _ OUTOF _ 10

9.0-21)4 _ 2MZMI351C IPWUCOI,4_s _ X L32 m 0.RRI FILM _ S,'N 5_52RANCE:G 1, 1 _ H 6, 4.ii _ A 8, 1.4,.1 4 8_Ez U21. 3

188.8

4_8

9 10 11 1213 14 1516" -J --- i ;- n" i j j

12_ 13e0 1488 1_ 1S88 I?N2_ee 21:4e 23:28 2:5:1le 26=48 28:28

J

IN38W 31s4e

1

TIJ'IE

Page 64: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

SI.D-2 #5 Compounds

Peak No._ Identification

1 Sulfur hexafluoride

Identified

RIC Value

12560

Conc (ug/g) Conc (,o/g)Meas. Corr.

0.237J2 Chlorotrifluoroethene 758784 14.3313 11,2-Dichloro-l,2-difluoroethene 162816 3.0754 BP 59, 43(65) 231680 0.679S6

BP 68, 42(55), 77(10)1,1,2-Trichloro-l,2,2-trifluoroethaneMethylene chloride

8 Trichiorotrlfluoroethane

5765122863100543744901120541696149248

9 BP43, 59(30)10 BP 75

1.58934.45910.27017.0201.5870.437

11 Methylcyclopentane 33600 0.09812 Silane 23840 0.07013 470528 1.440Benzene + Cyclohexane14 Cyclohexene15 Acetic acid16 Methylcyciohexane17 Toluene18 Xyiene or Ethylbenzene

Xylene

348167833618368

1815046944

1211256054936

19202122

BP 133, 151(60)StyreneDimethyffuranone

0.1020.2290.054

162..235

5.695

0.510 1.6210.0200.0350.0160.014

5560 0.016;23 Siloxane, BP 281 6250 0.01824 ;4-Ethenyl-1,4-dimethylcyclohexene 16544 0.04825 Substituted cyclohexane, BP 83, 125(55) 16704 0.049

8716826 0.255Methenamine

a Quantitation based on an actual standard compound.b Quantitation based on comparison to average of three halogenated standard compounds.

a

_bbC

C

C

C

a

c

c

_C

,C

C

C

C

C

C

c

C

c Quantitation based on comparison to average of three non-halogenated standard compounds.

Page 65: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

7

IM.O

TOTRL _ITAI 19B31E_Ol _ lira TO11_.1,,e54 14s'22lt CRI._s I_IICN.. I_ OUTI_" _ TO.TmlIPLEs_D-2_ _ 2 IIIH_IC 17'g_CONIC.s i_lq X L32 M L_U_ i_IJ11_X5 5_ 5_2I_ G 1o 1 LJ_ H Oo 4.0 gU_ R I° 1.8J il g_: U3, 3

is 1_

17

Ai

IIM16_q

D

,l_-m

20 25261819 2122 23 24 _' t

i i i i i

:3,sM 21:d 23=20 _sm _e,X_ 20=20

tam38:_

l

31=48

|SC_4TINE

Page 66: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

SLJ-I #1 Compounds Identfl'md

Peak No. identification RIC Value Conc (l_g) Conc (pgJg)Meas. Corr.

1 Bromotrifluoromethane 13344 0.297

1142

2 1,2-Dichloro-l_,2,2-tetrafiuoroethane 15863 Methylene chloride 184324 Acetic acid 96165 Toluene

0.0350A110.0450.004

IoIo

_C

0.011 _a6 Xylene or Ethylbenzene 1290 0.006 c7 2-Bmoxyethanol 3332 0.016 c8 Phenol + Benzaldehyde 2116 0.010 c9 Trimethylhenzene 1610 0.008 c

a Quantitation based on an actual standard compound.b Quantitation based on comparison to average of three halogenated standard compounds.c Quantitation based on comparison to average of four non-halogenated standard compounds.

Page 67: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

TOTAL DIiT_ _ OlIe/24/94 12zSIdM CAIJs IJ3MICAL ISSmIPI.FJ g,..klel SPt.FfI.I_ _ • 3_C l_qlM;CSID_s _ X 1.32 IM l,MM FIIJ_ lelX5 IMSC 15

G to_tlLO ....

rOTa.

LU .... L_L . -.aLJ ..... j -- -I "ll_

.... _-'--'T _r*- -:- +- ,_ -- +r-',411

Sill 6"41

SCI_S 211101111OUT CF" 2mTO_

| + H I,, 4.I Ilk A II, 1.11 J I _ Urn, 33

1

ha Uhm

t

4

7_ I I I8MM MII IIi

TOT_I. DI_Tm 1S84417el SC_4S 118M TO _MM811,,'24,,_1.121_:U CIV_: lJlB381CAI..IS OUT _ 2n TO 2888SN'I_Ee SL.._III SP_TI.£_ 2rllH I _ 171MOCONOS._Itn x 0.32 m z.S.II Irll.fl RTiC5[MSC IS

G 1, I I,_s 14 I, 4.41 _ A I, ?+.lIJ o _ U21, 3IN.O l?_

45- 21m

7 8 g

, m ' , , , , ,I 1 1411 1 IGm 17gg 1888 1_ SC:AH28:ee 21m4G 2gz28 _sB8 2G#40 28#28 30:_ 3t:4e Tile

Page 68: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

SLJ-I #2 Compound; Identified

Peak No. Identification RIC Value

2

4

Broml_:lifluoromethaneIDichlorodifluoromethane1,1,2-Trichloro-l,2,2.trifluoroethaneMethylene chlorideAcetic acid

160162336

54784321O24S40S72

conc(p g) ConcMeas. Corr.

0.239 b0.035 b0,441 0.823 a4.783 b1.701 c

a Quantitation based on an actual standard compound.b Quantitabon based on comparison to average of three halogenated standard compounds.c Quantitation based on comparison to average of four non-halogeni_,d standard Compounds.

Page 69: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

7OTN.. I_T_ _ tl10124,'94 11tSBtOO CALl: ]J3811_L 15

51.,_L82 SPt.ZTL[SS2N_ e _ 1"/88UCOHDS.: 6U't X L32 Im 1._ln F]lJ'l R'I_ 13BC ISINGEs G 1o I _ N O, 4.0 IIJ_t A Ib 1.OJ

•41.e .....

oiw.

5C2H5 280 TO llO00UTOF 280 1_0 20U

II_.s U:2So 3

4

lli.|

I

2

300 440 HI0 GJ8 788 _O 5lO 18185a 80 G148 k2B 1kin 11:4e 13s28 ISzgO 1Sat

i"OT_F,. _T_ ,t50486 Of _ lZm TO10_4J54 ll:_O_tO0 C_t.I: L58_IC_ _ OUTOF 208 TO

5_-182 5_'_$5 _ t_OC 178PJCI](Ls GIIIX L32 Nq I.SJI.I i:II.H RTX:5I_C 1S

G /., X L.q0fl.J N II, 4.8 g, NNs A II, 1.8J 0 _ U20, 32reelS.

45-

mI

__ _L_i -- "I l I ' "_ I

120g 1300 14N 1580 1GBO 1700_:_ 21:46 23:29 25:08 2S:4e 29:28

Ii31sm

lgqO31:48

4

TIME

Page 70: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

P_kNo.

SLJ-1 #3 Compound

Identification

Identif'md

Furan

5 Methylene chloride

6 3-methylpentane7 2-butenal

8 Benzene9 Acetic acid

10 Toluene

11 Xylene or Ethylbenzene

12 2(3H)-Furano .he

RIC Value conc (;_g)Mess.

Conc (;Jg/g)

1 BromoUifluoromethane . : ,1_'7i; 0.8922 Dichlorodifluoromethane 45120 0.903

3 1,2-Dichioro-t .1,2,2.tetmfluoroe_ha. ne 4944 0.0994 " ' 42624 0.180

COLT.

042080 18.857

SlSO o_o2433728 0.143

555521 0.203 0.802

36352 0,154

18528 0.055 0.175

8768 0.037_492 O.OlS

--LJ

13 Cyciohexanone 4608 " 0.01914 Hexanoic acid 9920 0.042

15 !Benzaideh.yde 28064 0.119 i16 Trimethylbenzene 4832 0.02017 Nonanal 6752 0.029

18 Benzoic acid 6688 0.02819

_a

2O

2t

60160 0.25411664 0.049

11808' 0.050

Capro_ctam1-Decanol

Dodecanoic acid

QuantitatJon based on an actual standard compound.

b Quantitation based on comparison to average of three halogenal_d'standard compounds."

c QuantJtation based on comparison to average of four nondmiogenated standard compounds.

b

b

c

b

c

c

s

c

a

c

_c,c

c

cc

c

c

c

c

c

Page 71: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

_lU.8

tOTAL

180.8

TOT_ I_T_ 19m1115OlCPLIs 1.q_OIG_,. 15

9,.J.-le3 SPLZI'LES32C_HOS.z 6m X 0.32 m hSJR FP,.H Im_ I]ESC ISIll_G_ G 1. I i.BIELa N 0.4.8 _ A

SCANS 2N TO 11mOUTOF 2N TO 2DN

L I.|J 0 _ U20o 3

5

1 42 3

300 418 _JO 6N5aeO Gsq |t_ lOsO0

5

J

llt44D 13_28

T_rAL ORTA: 1_8qi5 O! _ llW TO 200018,'24,,S4 11806s110 CRLIs lSB301C_L e5 OUT CF 200 TO

9,.J-le3 SR.ZTt.ESS2 elIHI3UCCONDS.: 6i X 8.32 I_ l.:Lm FIUI _ DESC ISItfg4_= C 1, I I.IUB.J X L 4.8 OUW41R li, 1.11J 6 BA_ U2L 3

8

A15ea

10--.J

45- 308

AI

15 19

11 121314_. 16 17 18 __ 20

1280 1380 14_ 1_88 1600 I;1'88 18m2Osm 21=4e 23_ 25:_ 26_4_ 28:28 3_110

21

31n4e _NE

Page 72: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Sl.J-1 #4 Compounck; Identified

Peak No. identification RIC Value Conc (pg/g) Conc (pg/g).-. Meas. Corr.

1 Bromotrifluoromethane 26336 0.56645504 0.9792 l_-Oichloro-l,l,2,2-tetmfluoroethane

Unknown, BP 41, 56(20)Unknown chlorofiuorocarbon

98176 0.4464 23424 0.504

5 Unknown, BP 45, 77(15) 121984 0,5546 Acetone 4.825 39.037

FuranUnknown, BP 45Methylene chlorideButanal2-MethylfuranTetrahydrofuran2-Butenal

789

101112

36198479360

Xylene or Ethylbenzene

588800711680

289281GO007352

58816401376

1314 Benzene15 1-Butanol .. 1049616 Acetic acid 5446417 Toluene 1505618 Methyi-(1H)-pyrrole 239619

styrenePhenol + Benzaldehyde

2O2122232425

92162308

2995250725264

MethyiphenolMe,myJ nzald hyde

0.3602673

15.3050.1310.0730.033o.2670.398 1.5720.081 0.2410.2470.048 0.1530.0110.0420.0100.1360.0230.024

Caprolactam 17696 0.080Unknown fatty acid 12368 0.056

a QuantitatJon based on an actual standard compound.

bbc

bC

a

C

_C

Io

C

a

a

c

a

c

c

c

c

cC

C

IC

b Quantitation based on comparison to average of three heiogenated'standard compounds, lc Quantitation based on comparison to average of four non-halogenated standard compounds.

C

Page 73: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

I'OTFL OAT_ 1_0404 el _ 200 TO 11m18,,,"_'4,,,"cJ4lexlSxM CALl- 1_0301CN.. _ CUT (F _ 10

gL..._-lt4 g%_ 2 him 31: 1_II8U(:_HOS.s mnx 0.321111 i.:w._ Fll.n R1_5 _ IS

G 1o I _ N I. 4.8 GRIn A O, 1.eJ 0 _ U28, 3

4.i.O .....

ITd_L

j 2

5aCe 6a_ Ibm

6

• 5 "8 i : o_lll-

l;m 7'O8 888l_m 11.40

14

13 _ 16

13:21 15:m

I'OTAL oA_rA: 190404 el SCANS 1188 TOlO/'k,£vg4 lkl_N CW.]: _ICW,. 15 gUT OF' 201 TO

g_,l-lN _l_ 2 I'.Ial _ I?WUC_n tall x IL32 I_ I.SUM FILN RTX5 _5C IS

G I, Z LP_: H a, 14.8 OUla_ A 8, I.B J 8 BI_SEsU 26, 3

180.0

I_40

45-300

n !

12N2e:ee

21

2223 24 25

13m 14e_ 1SEe IfAle I?UB IJ8 li S[_21:48 23:2B 25=08 25:441 28:28 _um 31:41) TIIqE

Page 74: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

SLJ-1 #5 Compound..

Peak No. Identification

1234

Bromoll:ifluoromethaneChlorotrifiuoroethenel-Propene

!1,2-Dichloro-l,l,2,2.tetratluoroethane$ 2-Butene6 1,2-Dichloro-l,2-difiuoroethene

; Identified

RIC Value Conc (pg/g) Conc (pg/g)Meas. Corr.

12256 0.2846688 0.155

16832 0.08246912 1.088

206848

89

10111213141516171819202122232425262728293O31

a

Acetone

1,1,2-Trichloro-l,2,2-trffluoroethaneMethylene chlorideIsopropyl alcohol2-MethylfumnSilaneTetmhydrofumnBenzene + Cyclohexane

Acetic acidMethylcyclohexaneToluene

.r,..Methyl-l-hepteneXylene or EthylbenzeneStyreneCyciohexanonePhenol + Benzaldehyde3-Methyl-2(SH)-furanoneLJmonene

MethylphenolBP 44, 57(68), 73(60)Benzoic acidBenzenepropanenitrileMethenamineCaprolactamAiiphatic alcohol

Quantitation based on an actual standard compound.

11920973034030156854272O

33066900

1.01 30.276

139.889 1131.79'3.783 17.810

12.5893547.509

55168 0.27035904 0.176

469776 2.251208128 0.88093056 t12208352543784

13008

75639.853

3.4520.4560.0600.122 0.3860.0190.064

7640 0.0376312 0.031

19424 0.09514384 0.0704400

10O322112057043628

19712

0.0220.0490.1030.0280.0180.0970.1830.071

3731214528

b Quantitation based on comparison to average of three halogenated standard compounds.

bbC

bC

rba

a

ba

c

c

c

a

c

c

a

c

c

c

c

c

c

c

c

c

ic

c

c Quantitation based on comparison to average of four non-halogenated standard compounds.

Page 75: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

4eo.$

'OTAL

TOTAl. I_T_ 188413 el1e,,,24.,_ 8,40#00 C_..;: I_ICAL._I.IPLE_ 9,.J-le5 sR.r'II.ESS 2 _H¢ 35eC I;'WV001406.. 6111X I.. "n _l I._JH I_Lel Itl"_ OESC 15

1

1, 1 _s H I, 4.11 _ A O, 1.8J il BASE: U28, 3

9I 7 10

,_bs

& J 12 15 17

_*m 6#441 M_ IixW llz.'le 13:28 15:M 16s411

lile.O

TOTAL I_TA1 198403 Ol SCAt6 lira 10 2NO1B,'24,,'_ 8sOelO CALII I_IC_. 15 OUT OF 200 TO2000SillIR.Et 9,.J-le_ _ 2 _ 3mC 1"/1_/C0_5.: $1flX 8.3271'1 l._fl FILfl RT_ W3C ISIim_z G |, 1 _ N $o 4.80U_# A 8, 1.8J il _ U21, 3

SS9424.

,L_- 3ee

29

I++ m .:,+ +,5 .26 m+s+.4 i + - " " '+ - _ - -"-" 1 | l i " I ]

_8:Oe 21: 40 23a_ 23: m 26=4e 2g*28

31

3B:m 31s,W TZME

Page 76: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

P-l-STS.58 Compounlls Identified

Peak No.

2

Identification

Bromo:.;;;uo_,:._._hane!1,1-Dichloro-l,l,2,2-tetrafluoroethaneMethylene chlorideBenzenel-Hydroxy-2-propanoneTolueneXylene or Ethylbenzene

RIC Value Conc (,g/g) Conc (pg/g)lt_e:_s. Corr.

_/a6 0.004 b1542 0.025 b4472 0.073 b2980 0.008 0.015 a3604 0.008 c1640 0.002 0.007 a3.1.46 0.007 c

a Quantitation based on an actual standard compound. Ib Quantitation based on comparison to average of three halogenated standard compounds. l

c Qua.titation based on comparison to average of four non-haiogenated standard compounds.

Page 77: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

tOTal.4

6

_ _¥_ _ 81 _ llN TO11_ 141_ as _: _ _ _

PI _ 2"1_ 3OOC

G 1, t I_ N 8, 4.0 au_ A II, l.|J It _ U28, 3

tn.| 7728.

7

Page 78: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

P-2-STS-58 Compounq

Peak No. Identification

1234567

9101112131415161718192O2122

Dichlorodifluoromethane

1,2-Dichloro-l,l,2_2-telmfluoroethaneUnknown, BP 43, 77(20)Methylene chlorideAcetic acidBenzene

l-Hydroxy-2-propanoneTolueneXylene or EthylbenzenestyrenePhenol

Ben=aldehydeBenzonitrileTrimethyibenzeneBenzeneacetaldehydeMethylphenolrBenzeneacetonitriieNaphthaleneBenzenepropanenitrileHydrocarbonMW 134f substituted benzeneMethylbenzonitrile

a Quantitation based on an actual standard compound.

Is Identified

RIC Value Conc (Pg/o) Conc (1_1_i)MeaLs. Corr.

1164 0.0167144 0.098

84864 0.15310656 0.1455744 0.01011536 0.0265904 0.0118352 0.011552O 0.0104512 0.0086048 0.0112928 0.005_1980 0.0042668 0.0052792 - 0.0055248 0.0092600 0.0052696 0.0054184 0.0085664 0.0103960 0.0077680 0.014

0.048

0.032

b Quantitation based on comparison to average of three halogenated standard compound_s_c

bbc

bC

_a

c

a

c

Quantitation based on comparison to average of four non-halogenated standard compounds.

C

C

C

C

C

IcIC

C

C

C

C

Page 79: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

TOTAL11AJT_J4 14153a00SAFPL_, P2 5PLTrLESS 2 RIla t 3_CCOHD_: _ X 8.32 Im 1.3U5 FILH RIX5 _SC ISNN4GE_; 1, I LIBJ H e, 4.8 Gtaql4s A 0,

4OO.O .... 3

• TnL 2

I_TA: 158718 Ol SC_tS 20e TO 11NCnt.Z: I.qO381C_L 05 OUT OF 288 TO2800

.OJ 0 8ASEJ Urn, 3

4 G

' J " I " I ' I ' i ' I

5,08 S:4e 8:20 le:OO 11a40 13a28 15am 1Gsq

TOTAL O¢ITA:158710 01 _ 1108 TO _BM1147154 14:53:m CN..I:158381CN. 05 OUT OF 200 TO 2080._ p2 SPLI'_.I[SS 2 _H | 3_C014115.m_ X 8.32 m I.SuHFILM RIX5 I]E3CIS

G I, I 1.qEB.:H 0, 4.00UNi: # e, 1.0- O 8#SE: u28, 3

tOQ.O

11

9

10

16

I 1e2o

;2 14 1151 • 17 1, i ti 1

3_

| l ! I I I I I1 13m 14m 1508 1600 17_ 1888 lgeOZ2e_M 21:4e 23=20 25,88 28:4e 28:219 30 08 31=40 TIME

Page 80: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

P-3-STS-58 Compoun Is Identified

Peak No.

234

Identifi.c.aUon

Methylene chlorideToluenexy|eneor Etn_n_ne

RIC Value

270423841110

Conc (pala)Meas.

0.0000.0030.000

Benzaldehyde 1014 0.000

Conclr,io/o)Corr.

boioos.,a

a Ouantilation based on an actual standard compound.b QuanUtation based on compariso n to average of three halogenated standard cmnpounds.c Quantitafion based on comparison to average of four non-haiogenated standard compounds'.

C

¢

Page 81: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

188.8

308 4410 _J8 600 718 08O 5e0 18N5t00 6:40 8a20 lkO0 Ltoq 13t_ lSxm IGs40

TOTN. OAlfi; 1_711 01 _ lira TOIL_lJT,,'54 16:_:m CIL..I: I_IS?8|C;_L J_, GUT OF 288 TO5N5:5._ P3 5P,.Z'fU_; 21tiNt 350CC_84_.: GOItX L32 Nq 1._115 F_LJqIt'T'_ OESC ZSRPMGF.zG 1, I _= H 0o 4.8 GU_s _ 8, l.JJ 8 _ltz U_, 3

3143B.

,_,- 388

3 ,t

12m 1300 1400 1SIm i fag20:8e 21:40 23=5a 25sin 2GJ4O

, ,, ",

I;, 1;,_Ot20 30100 31s40

J

5C114TIJqE

Page 82: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

AW-1-STS-58 CompouJtds Identit'md

Peak No.

1234

identification RIC Value

lt2-Dichloro-l,l_2-CetmfluoroethaneTric hiorofluoromethane1,1_-Trichloro-l_,2-trifluoroethane

IMethylene chlorideAcetic acid

Conc (,g/g) Conc (pg/g)Meas. Corr.

35008 0.3854600 0.0624360 0.027

227328 2.4985 110720 0.160$ Benzene 5800 0.0107 Toluene 2060 0.0028 Xylene or Ethylbenzene

Styrene910

1084 .....0.00291S , o.oo,I

o.oo2Benzaldehyde

Ib0.143 a0.051 ;a

bC

0.019 a0.004 a

C

c

C

a Quantitation based on an actual standard compound.b Quantitation based on comparison to average of three halogenated standard compounds.c Quantitation based on comparison to average of four non-halogenated standard compoun¢Js.

Page 83: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

OTAL

1 S

108.8

2 3

T_AL _TA:. _e;'Z2 t_ _ :Zm TO2m8

.5_l'ff_.,EtAJ41SPLI_ ;_111,483S8CCOHOS., 60el X L32 IS5 I._UI5 FILn _ OESC 15J_NG_G 1, ! L,qBB.a N 8o4.e G,W_A O, X.JJ 8 BAS_U3, 3

8 9 10

131 1,18 l_le tl;OI 171020s80 21:40 23m20 2_:00 2Sn4e 20,28

10N30:88 31:4e

5_mT_I'E

Page 84: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

AW-2-STS-58 Compoui _ds Identified

Peak No.

2

Identification

11,2-Dichloro-1,1,2,2.tetrafluoroethane

_Methylene chloride

RIC Value

47552131840

1.1283.128

3 Acetic acid 134144 0.363456O3584

4 Toluene

5 Phenol + Benzaldehyde

a QuantitatJon based on an actual standard compound.

0.0100.010

Cone (pg/g)Corr.

EbbC

0.021 a

Ib Ouantitation based on comParison to average of three halogenated standard compounds.c Quantitation based on comParison to average of four non-halogenated standard compounds.

Page 85: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

11,,88,,$4 llslSsm C_L.Is ISSNICIL. OGSApPI.Ex JM2 gq.l'Tl.l_SS 2RIHB "_CI]4DS.x Sin x 8. ''n I!t I.SUI'I IC'll.l'lL'T'_5 CESC IS

G t, I _ H II, 4.8 eU/Ms n l, l.IJ I

400.0 ....

211 '_0 llOI_U'T 0:" "_ TO 2NO

_Ua, $

2 3

I'OT& _qTfh 19m13 QI _ lib TO11_ llsl$:gO Clrl_: I_IC_L _ OUT OF' _ TO

_ SPI.z'r,.£SS _XNtC:CHDS.,601t x 0,32 I_ I._UR FII.M _ CESC ISll_Ea C 1, 1 l.ll_.s 14 an, 4.8 _ A tl, 1.8J 0 _ U29, 3

IM.O

,1_- :Am

_ __ , L .

_m

s

l _ -; ]

21s_ _ 25:M 2_:46 28s28

! - !

30:.00 3t:q Till(

Page 86: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Peak No.

3

4

5

AW-3-STS-58 Compou

identification

1 r2-Dichloro-t,l,2_2-tetrafluoroethanerMethylene chlorideiChloroform

Acetic acid

_ds Identif'm(_

Phenol + BenzaidehydeLimonene

RIC Value Conc (pglg)Meas.

23136 0.647

16102435455¸

176640

3024

4.504

0.9920.563

0.010

6 4904 0.016

a Quantitation based on an actual standard compound.

Conc (go/g)Corr.

b

c

cc

b Quantitation based on comparison to average of three halogenated standard compounds.c Quantitation based on comparison to average of four non-halogenated standard compounds

Page 87: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

2

ILs4e

TI31"_L DATAa 190004 el _ 1188 TeD

nit3 S_t..ZTL£SS 2l_II4135eCC_o_5. j SOPJx L32 _ 1.2l_ FIU_ _ _ESC LSI_£E, G t, i _ )4 6, *,.ll _ A o, t.i J O B_ U20, 3

|T |

4S- 300

S 6

12R 13m 1400 1_ t_ 1700 10N l_ SC_20,00 21:_ 23:20 2_,:_ 2S:40 28s20 30=.00 31:44) T2_

Page 88: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

ACT-l-STS-58 Compo, mds identifie

Peak No.

1234

Identification RIC Value

l-propenel_2-Dichloro-l,lt_2.tetrafluoroethaneAcetaldehydeEthanol

5 Acetone6

101112

Isopropanol

Methylene chlorideTetrahydrofuranBenzene + Cyclohexanel-ButanolAcetic acid

1-Hydroxy-2.t)ropanoneToluene13

Conc (p_'g) Conc (pglg)Meas. Corr.

112384 O.275175872 3.779206848265216779844865040_314880

4896131201.1328184326480

0.5072.6957.970

55.9726.7660.0120.0330.0770.0450.0160.013

C

bC

b Quantitation based on comparison to average of three halogenated standard compounds.c Quantitation based on comparison to average of four non-halogenated standard compounds.

64.484 a1193.428 a

bC

0.131 a0:__ a

IC

=C

0.041 a

a Quantitation based on an actual standard compound.

6600

82.151 al

Page 89: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

.40O.0

188.8

TOT_ Offtle _ it _ 200 70 llmLI/II6,'_ l_,4_m (3_.I: 1._ilC31b 04; OUTOF 288 TO_Ifl.Es _CTI SPI.I'ILES5 _ 3mCCQNDS.s 6111X 8.32 I_ 1.SUn F2LIqRI_ O_C t¢

5 7

6

/13

743424.

45-389

TIME

Page 90: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

,.P_kNo.

1

2

34

5

6

78

9

1011

12

13

14

1616

17

18

19

2021

22

23

24

25

26

ACT-2-STS-,58 CompoUnds identifie,

Identification RIC Value

122496

! t.2-Dichloro-1 rl r2_2-tetrafl uoroethane

:AcetaldehydeEthanol

Acetone

Methylene chlodda

isopropanolBenzene + Cyclohexane

1-hepteneUnknown, silane BP 77v 45(30)Toluene

N,N.DimethylformamideTetrachloroethene

Xylene or Ethylbenzene

Unknown, BP 133_ 151(70)}O-Xylene

;Siloxane vBP 281C3-Benzene

Tdmethylbenzene2-Ethyl-l.hexanolSiloxane

Hydrocarbon

HydrocarbonSiioxane, BP 73, 267(40)Methenamine

Caprolactam

174592

Conc (m/g)Meas.

0.2753.442

71296 0.160

127744 1.191

3496600 32.785

388608 7.6612332710

173056

53824

241200429568

31968

31424

25600i

596992145448

1470450

334O8

4224O279O40

3036165"7216

32768

ia Quantitation based on an actual standard compound.

615424

52572

57920

138.4590.400

0.121

0.547 _0.768

0.0720.619

o.ossI1.342i

Conc (pg/g)Corr.

36.300

265.248

2952.4331.583

2.442

0.109 t

3.3060.075

0.095

0.627

0.663

0.129

0.074

1 384

0.1180.130

b Quantitation based on comparison t 9 average of three halogenated standa_ compounds.c Quantitation based on comparison to average of four non-halogenated standard compounds.

C

Ib

18

_b

a

a

C

C

a

C

b

C

C

C

C

C

C

¢

C

Lc_C

!C

C

C

Page 91: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

_408.8

TOTAt. OATAml.qo88G 0111s08_4 t3:30:N CALl: 158001CAL 06

_T2 SPL._.J_S 251m _8CCOHOS.: SSn X L22 m |o_Un I_U5 r/x5 _ IS

G 1, I _ N Oo 4.0 _ A e, 1.eJ

SCAHS 200 T0 1100GUT_ 2003'02800

8 _u '_, 3

rOTRL

180.8

5ago

I " J " I

4gg _ 6886m_ h_ llhN

6

5 7

11

8 10 d

lltW 13128 ISti l_m40

_L OATIt_ li el 5C_5 1108 TO2888

CCHOS.xanx 8.321,11 1.1H RuJI RI_ I]ESC ISIMHE, (; 1, 1 _ N eo 4.8 _ R tb, L.SJ 0 BJ_F.t U20, 3

2736128.

17

1S

1280 130028tm 21:48

45-m

24

20,t8 192_i 22 23 t. 2528

1400 1_10 l_ 11tl 1880 _23:28 25tM _.40 281_Ii 31hm 31|40 TIME

Page 92: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

ACT-3-STS-58 Compo mds identif'mJ

Peak No. Identification RIC Value Conc lug/o)Meas.

Conc (IJg/g)Corr.

1 l-Propene 1479682 I t2-Dichlo .ro-1_1,2T2-tetrafl uo.ro_hane 50880 1.4433 Acetaldehyde 173824 0.5624 Propane 281600 0.9115 Ethanol 498688 6.689 203.9166 Acetone 8449090 113.996 922.3007 Methylene chloride 324096 9.1948 Isopropanol 9250290 790.140 16847.335

9 Tetrahydrofuran 60926 0.19710

0.479

22464 1.642 10.4261l_l_l-Trichloroethane11 Hydrocarbon 22784 0.07412 Benzene + Cyclohexane 84736 0,?.82 1.11613 1-Butanol 64832 0.579 1.734

14 Hydrocarbon 29664 0.09615 Acetic acid 42176 0.136

16 l-Hydroxy-2-propanone 13760 0.045.117 Toluene 189952 0.489 1.554

C

bC

C

a

a

ba

c

a

c

a

a

_c

:c

c

a

18 Tetmchloroethene 10656 0.302 b19 N_N-Dimethylformamide 10608 0.034 c20 Xylene or Ethylbenzene 6632 0.021 c21 Xylene or Ethylbenzene 20832 0.067 c22 Styrene + N_N-dimethylacetamide 8384 0.027 c23 O-X¥1eue 6040 0.020 c24 Phenol + Benzaldehyde 8832 0.029 c25 2-Ethyi-l-hexanol 15808 0.051 c26 Hydrocarbon 9792 0.032 c27 IUnknown wBP 69t 81(50) , 25152 0.081 c

a Quantitation based on an actual standard compound.b Quantitation based on comparison to average of three halogenated standard compounds.c Quantitation based on comparison to average of four non-halogenated standard compounds.

Page 93: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

rOTAL1

TOTeL _T_ _ 0! S;CmSIlm TO 2NO11,t6/94 14,21t00 CALl: 138N1(:_L lIG OUT IF 200 TO 2N0

_ Si,._TLE55 _ltNIl_0CC2]H[_.n 61.1X i1.22 Be },.ZMq FIIJI _ D£5C ISI_ G 1, ! _ H e, 4.11 ouM Pl O, 1.0,J o _ u'J'n, 3

IN.a 2183168.

45- 3OO

1819 20212223 24 25 26

1200 13Be 1400 I_N I_N 1"_0 ]Jle 1_1021hoe 21:4e 23;120 2_8(!e 2Et4e 28a2B 38:.N 31:441 TIME

Page 94: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

Peak No.

123

ACT.4 -STS-55 Compo

Identification

101112

111-Dichioro-1 _._.r2-tetmtluoroethanePropaneEthanol

4 Trichlorofluoromethane5 Acetone

Methylene chlorideIsopropanol

111r1-TrichloroethaneBenzene + Cyclohexane

!l-ButanolAcetic acid

1-Hy_roxy-2-propanone13 Toluene14 Tetrachloroethene1516171819

NtN-DimethylformamideXylene or EthylbenzeneHydrocarbonHydrocarbonUnknown BP 69, 81(55)

rods Identif_ d

RIC Value Conc (pg/g) Cone (pg/g)Meas. Corr.

12172863616

3.9190.2348.697 265.1643.277 19.481

57139274624

1930800272384

29.565 239.1968.769:

113_294 2415.6470.463 2.937

11687005576

21984 0.083 0._2929280163206416:

3744039685112

0,2970.0600.0240.1090.1280.019

3380 0.01216384 0.0601654421184

0.0610.078

0.889

0.348

a QuantJtation based on an actual standard compound.b Quantitation based on comparison to average of three halogenated standard compounds.c Quantitation based on comparison to average of four non-halogenated standard compounds.

bC

a

a

a

ba

a

laa

c

c

a

rbC

c

C

c

lc

Page 95: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

41.8

'0T_L

lm.O

TOTAL _ l_ el _ _TO tlm1L/_6,'94 15s0BsM CN.Xs I_m|C2L 16 OUT OF 2m TO 2NO.TNIPL_ _'T4 _ 21_mCI)N05., lair X e.',_ el'l l.mJel FlLei It'll5 I]ESC IS

G 1,. I _ N i. 4.0 GIUAmA

!

1 4

0, 1.0J $ E_q_J U2L. 3

t'

8

TOT& 01_k 15Nm 01 _ fin TOII.,'W.,_ l_10sN I_f_: L_mllO_L !_ OUTCF _ TO 2NO

ACT4 Siq..'TLESS_lNICOHD_s 681'1X 11.3_ ell I._H FILll RIX5 I]ESC ISIMHG_ G 1, 1 1.40G_ H II, 4.11 UHs A |, 1.8J 8 iil_JU28, 3

1113

|

m16.

45- 31m

1415

I

16

'- -- i . 7 i" ' 0 ' iL290 13N 1_ 1"mm IEU28n88 21:4e 23:_ 25s00 2Ga4e

17 18A .... |

19

1elm 130:n 31:q TIME

Page 96: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

PeakNo.

1

23

4

5

S7

6

9

10

11

12

ACT-5-STS-58 Compol ands Identit'ml I

Identification RIC Value

1-Propane

I r2-Dichloro-1 r1,2_2-1mtrafi uo roethane

AcetaldehydePropaneEthanol

Tnchlomfluoromethane

Acetone

Methylene chloride

Isopropyl alcoholTetrahydrofuranFormic acid

Benzene + Cyclohexane13 1-Butanol14 Acetic acid

15 Toluene

16 NrN-dimethylformamide

4-Methylpentanenitrile

Xylene or EthylbenzenePhenol

101632

142336

Conc (pg/g) Conc (IJglg)Mess. COLT.

0.400

4.914

17

1819

20

21

22

23

242176 0.954167424 0.659

410624 6.702 204.3391416768 19.624 116.670

4300910 70.619 571.351

293888 10.1461033260 107.409

19168 _ 0.075

10384 0.041

183040

2290.161

76032

36592

0.741 2.9330.826 2.474

0.152

138752 0.435i 1.3828736 0.034

5032 0.020

5384 0.021

5280 0.021

3-Methyi-2(SH)-furanone 4536 0.018Nonanal 3776 0.015Decanal 4568 0.018

88641 0.035Methenamine

.a Quantitation based on an actual standard compound.

b Quantitation based on comparison to average of three halogenated standard compounds.c

cb

Quantitation based on comparison to average of four non-halogenated standard compounds.

c

c

c

c

8

as

b

a

Ic

c

a

ac

a

c

c

c

cc

c

Page 97: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal

IOLO

TOTAL Dnl_. 1_ e!

_ _,_ 2 holt 3mC

_r_ 1, 1 _N e. 4.e _ A $o 1.8j o

7

I

2

3

SC_H5 2BO TO liraOUT 1)_ 2W TO 21

9

_15 SPLm.E_ 2 Pllm 31C

G 1, 1 _ N 8, 4.8 _ A 8, 1.8 J e _ u_, 3

12

13

14

15sW1888

_m

"m16 17 18 19 20 21_ _ 22 _. __

-- .. .

1_ 13m 1408 15m II_8 17g0 IOllO20sin 21:q 23t_i 25_m 26s4e 28128 3e:m

I I

ISlm31m4o TIRE

Page 98: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal
Page 99: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal
Page 100: Spacelab Charcoal malyses - Phase 1I - NASA overcome this problem, ... EI, 70eV @ 0.35 ma 29 to 300 Da, ... current in the background subtracted mass spectrum for the spiked charcoal