april 25,1991 reference no. 2141 · united states environmental protection agency region ix 75...
TRANSCRIPT
Consulting Engineers
April 25,1991
SFUND RECORDS CTR
88015060
CONESTOGA-ROVERS & ASSOCIATES LIMITED 651 Colby Drive, Waterloo, Ontario, Canada N2\ (519)884-0510 ^^^^^ RECORDS CTR
0222-00498
Reference No. 2141
Mr. Tom Dur\kelmari (H-7-2) Remedial Project Manager United States Environmental Protection Agency Region IX 75 Hawthorne Street San Francisco, California 94105
AR073S
Dear Mr. Dunkelman:
Re: Quality Assurance/Quality Control (QA/QC) Procedures Soil Gas Survey Hassayampa Landfill Site
Enclosed please find three (3) copies of the above referenced QA/QC procedures received from Tracer Research Corporation. We are submitting the procedures for your review and comment, but are aware that Tracer has previously completed soil gas surveys at a number of Region IX sites using these protocols.
If you have comments or questions, please direct them to the undersigned prior to May 6,1991, the scheduled start date for the survey.
If you have any questions, please do not hesitate to contact us.
Yours truly,
CONESTOGA-ROVERS & ASSOCIATES
( ^ ^ Steve M. Quigley, P. Eng. ^ ^ SMQ/pse/8
C.C. Hassayampa Technical Committee (w/o attach.) J. Sherard - Tracer (w/o attach.) B. Victor - Errol L. Montgomery & Associates (w/o attach.)
TRACER RESEARCH CORPORATION'S SAMPLING PROCEDURES
AND QA/QC PROCEDURES
PREPARED BY
ER RESEARCH CORPORATION
T r a c e r Resea rch C o r p o r a c i o n
SOIL GAS SAMPLING PROCEDURE
L Probe Placement
A) A clean probe (pipe) is removed from the "clean" storage tube on top of the van.
B) The soil gas probe is placed in the jaws of hydrauUc pusher/puller mechanism.
C) A sampling point is put on the bottom of the probe.
D) The hydraulic pushing mechanism is used to push the probe mto the ground.
E) If the pusher mechanism will not push the probe into the ground a sufficient
depth for sampling, the hydrauhc hammer is used to pound the probe into the
ground.
n. Sample Extraction
A) An adaptor (Figure 1) is put onto the top of the soil gas probe.
B) The vacuum pump is hooked onto the adaptor.
C) The vacuum pump is turned on and used to evacuate soil gas.
D) Evacuation will be at least 30 seconds but never more than 5 minutes for
samples having evacuation pressures less than 15 inches of mercury.
Evacuation times will be at least 1 minute, but no more than 5 minutes for
probes reading greater than 15 inches of mercury.
E) Gauges on the vacuum pump are checked for inches of mercury.
1. Gauge must read at least 2 inches of mercury less than
maximum vacuum to be extracting sufficient soil gas to collect
a vahd sample.
in. Sample Collection
A) With vacuum pump running, a hypodermic syringe needle is inserted
through the silicone rubber and down into the metal tubing of adaptor
T r a c e r Resea rch C o r p o r a c i o n
UL
(Figure 1).
B) Gas samples should only contact metal surfaces and never contact
potentially sorbing materials (i.e., mbing, hose, pump diaphragm).
C) The syringe is purged with soil gas then, without removing syringe needle
from adaptor, a 2-10 mL soil gas sample is collected.
D) The syringe and needle are removed from the adaptor and the end of the
needle is capped.
E) If necessary, a second 10 mL sample is collected using the same
procedure.
IV. Deactivation of Sampling Apparatus
A) The vacuum pump is turned off and unhooked from the adaptor.
B) The adaptor is removed and stored with equipment to be cleaned.
C) Using the hydrauhc puller mechanism, the probe is removed from the ground.
D) The probe is stored in the "dirty" probe tube on top of the van.
E) The probe hole is backfilled, if required.
V. Log Book and U.S. EPA Field Sheet Notations For Sampling (Figures 2A-2D)
A) Time (military notation)
B) Sample number (use client's numbering system)
C) Location (approximate description - i.e., street names)
D) Sampling depth
E) Evacuation time before sampling
F) Inches of mercury on vacuum pump gauge
G) Probe and adaptor numbers
H) Number of sampling points used
T r a c e r Research C o r p o r a c i o n
I) Observations (i.e., ground conditions, concrete, asphalt, soil appearance,
surface water, odors, vegetation, etc.)
J) Backfill procedure and materials, if used.
VI. Other Recordkeeping
A) Client-provided data sheets are filled out, if required
B) Sample location is marked on the site map
vn . Determination of Sampling Locations
A) Initial sample locations will be determined by client (perhaps after
consultation with TRC persoimel) prior to start of job.
B) Remaining sample locations may be detennined by:
1) CUent
a) Entire job sampling locations set up on grid system.
b) Client decides location of remaining sample
locations based on results of initial study, or
2) Client and TRC Personnel
a) Client and TRC persoimel decide location of
remaining sample locations based on results of
initial sample locations.
T r a c e r R e s e a r c h C o r p o r a c i o n
ANALYTICAL PROCEDURES
I. Varian 3300 Gas Chromatograph
A) Equipped with Electron Capture Detectors (ECD), Flame Ionization
Detectors (FID), Photo Ionization Detectors (PID) and/or Thermal
Conductivity (TC) Detectors.
B) The chromatographic column used by TRC for the analysis of halocarbons
is a 1/8" diameter packed column containing Alltech OV-101. This nicely
separates most of the tri-chloro and tetra-chloro compoimds that are
encountered in soil gas investigations. The di-chloro compounds tend to elute
ahead of the tri-chloro and tetra-chloro compounds, thus creating no
interference. In the event that assurance of the identity of a compound in
any particular sample is needed, it will be analyzed on a SP-1000 column
after the OV-101 analysis.
n. Two Spectra Physics SP4270 Computing Integrators.
The integrators are used to plot the chromatogram and measure the size of
the chromatographic peaks. The integrators compute and record the area of
each peak. The peak areas are used directly in calculation of contaminant
concentration.
m. Chemical Standards From ChemServices, Inc. of Westchester, Pennsylvania.
A) TRC uses analytical standards that are preanalyzed, of certified purities
and lot numbered for quality control assurance. Each vial is marked with
an expiration date. All analytical standards are the highest grade available.
Certified purities are typically 99%.
B) The Quality Assurance procedures used by ChemService were described
by the Laboratory Supervisor, Dr. Lyle Phipher:
T r a c e r R e s e a r c h C o r p o r a c i o n
1) The primary measurement equipment at ChemServices, the
analytical balance, is serviced by the Mettler Balance Company
on an annual basis and recalibrated with NBS traceable weights.
2) All chemicals purchased for use in making the standards are
checked for purity by means of gas chromatography using a
thermal conductivity detector. Their chemicals are purified as
needed.
3) The information on the purification and analysis of the
standards is made available upon request for any item they ship
when the item is identified by lot number. All standards and
chemicals are shipped with their lot numbers printed on them.
The standards used by TRC are made up in a two step dilution
ot the pure chemical furnished by ChemServices.
rv. Analytical Supplies
1. Sufficient 2 and 10 cc glass and Hamilton syringes so that none have to
be reused without first being cleaned.
2. Disposable lab supplies, where appropriate.
3. Glassware to prepare aqueous standards.
4. Miscellaneous laboratory suppUes.
T r a c e r Reaearch C o r p o r a c i o n
QA/QC PROCEDURES
L Standards
A) A fresh standard is prepared each day. The standards are made by serial
dilution.
1) First, a stock solution containing the standard in methanol
is prepared at TRC offices in Tucson. The stock solution is
prepared by pipetting the pure chemical into 250 mL of
methanol in a volumetric flask at room temperature. The
absolute mass is determined from the product of volume and
density calculated at room temperature. Hamilton microUter
syringes, with a manufacturer's stated accuracy of + or - 1%,
are used for pipetting. Informafion on.density is obtained from
the CRC Handbook of Physics and Chemistry. Once the stock
solution is prepared, typically in concentrafion range of 50-1000
mg/L, a working standard is prepared in water each day. The
solute in the stock solution has a strong affinity to remain in
methanol so there is no need to refrigerate the stock solution.
Additionally, the solute tends not to biodegrade or volatilize out
of the stock solution.
2) The working standards are prepared in 40 mL VOA sepmm
vials by diluting the appropriate ug/L quantity of the standard
solution into 40 mL of water.
B) The standard water is analyzed for contamination before making the
aqueous standard each day.
C) The aqueous standard is prepared in a clean vial using the same syringe
each day. The syringe should only be used for that standard.
T r a c e r Research C o r p o r a c i o n
D) Final dilution of the calibration standards are made in water in a VOA
vial having a Teflon coated septum cap instead of in a volumetric flask in
order to have the standard in a container with no air exposure. The VOA
bottie pennits mixing of the standard solution and subsequent syringe
sampUng all day long without opening the bottle or exposing it to air. The
measurement uncertainty inherent in the use of a VOA bottle instead of a
volumetric flask is approximately -t- or - 1%.
E) The aqueous standard will contain the compounds of interest in the range
of 5 to 100 ug/L depending on the detectability of the individual components.
The standard will be analyzed at least three times at the begirming of each
day to determine the mean response factor (RF) for each component (Figure
3). The standard wiU be injected again after every fifth sample to check
detector response and chromatographic performance of the instnunent
throughout the day.
F) The RF allows conversion of peak areas into concentrations for the
contaminants of interest. The RF used is changed if the standard response
varies 25%. If the standard injections vary by more than 25% the standard
injections are repeated. If the mean of the two standard injections represents
greater than 25% difference then a third standard is injected and a new RF
is calculated from the three standard injections. A new data sheet is started
with the new RF's and calibration data.
% difference = A area - B area
A area
Where ; A = mean peak area of standard injection from first caUbration
B = peak area of subsequent standard injection
G) The low ug/L aqueous standards that are made fresh daily need not be
refrigerated during the day because they do not change significantly in a 24
T r a c e r Reaearch C o r p o r a c i o n
hour period. On numerous occasions the unrefrigerated 24 hour old
standards have been compared with fresh standards and no difference has
been measurable. If the standards were made at high ppm levels in water,
the problem of volatilization would probably be more pronounced in the
absence of refrigeration.
H) Primary standards are kept in the hotel room when on a project.
I) A client may provide analytical standards for additional calibration and
verification.
n. Syringe Blanks
A) Each uL syringe is blanked before use.
B) 2 cc (glass) syringes wiU each be blanked if ambient air concentrations are
elevated (greater than or equal to 0.01 ug/L) for components of interest.
C) If ambient air concentrations are < 0.01 ug/L for components of interest,
a representative sample of at least two syringes are blanked at the beginmng
of each day. If representative syringes have no detectable contamination
remaining syringes need not be blanked. If any of representative syringes
show contamination, all 2 cc syringes must be blanked prior to use.
D) Syringe blanks are run with air or nitrogen.
E) If it is necessary for any syringe to be used again before cleaning, it is
blanked prior to its second use.
in. System Blanks
A) System blanks are ambient air drawn through the probe and complete
sampling apparatus (probe adaptor and 10 cc syringe) and analyzed by the
same procedure as a soil gas sample. The probe is above the ground.
B) One system blank is run at the begirming of each day and compared to
a concurrently sampled air analyses.
_
Tracer Reaearch Corporacion
C) A system blank is run before reusing any sampUng system component.
rv. Ambient Air Samples
A) Ambient air samples are coUected and analyzed a minimimi of two times
daily to monitor safety of the work environment and to estabUsh site
background concentrations, if any, for contaminants of interest.
B) All ambient air samples shall be documented (Figure 3).
V. Samples
A) All unknown samples wfll be analyzed at least twice.
B) More unknown samples will be run until reproducibility is within 25%,
computed as follows:
Difference = A - B (A + B)/2
Where; A is first measurement result
B is second measurement result
If the difference is greater than .25, a subsequent sample wiU be run until two
measurements are made that have a difference of .25 or less. Those two
measurements will be used in the final calculation for that sample.
C) The injection volume should be adjusted so that mass of analyte is as near
as possible to that which is contained in the standard, at least within a factor
of ten.
D) Whenever possible the attenuation for unknown samples is kept constant
through the day (so as to provide a visual check of integrations).
E) A water plug is used as a ga^ seal in uL syringes
F) A seal is established between syringes when subsampling
G) At very high concentrations air dilutions are acceptable once
concentration of contaminants in air have been estabUshed.
T r a c e r Researeh C o r p o r a c i o n
H) AU sample analysis are documented (Figure 3).
I) Separate data sheets are used if chromatographic conditions change
J) Everything is labeled in ug/L, mg/L, etc. PPM and PPB notations are to
be avoided.
VI. Daily System Preparation (Figure 4).
A) Integrators parameters are initialized
1. Pt. evaluation
2. Attenuation
3. Peak markers
4. Auto zero
5. Baseline offset (min. 10% of fuU scale)
B) The baseUne is checked for drift, noise, etc.
C) System parameters are set.
1. Gas flows (Note: Nj, air, H^ tank pressure on Page 1 of
chromatograms).
2. Temperatures
a) Injector
b) Colunm
c) Detector
D) After last analysis of the day conditioned septa are rotated into injection
ports used during the day and replaced with fresh septa.
E) Column and injector temperatures are run up to bake out residual
contamination.
F) Syringes are cleaned each day
1. 2 and 10 cc syringes are cleaned with Alconox or equivalent
detergent and brush
10
T r a c e r Research C o r p o r a c i o n
2. uL syringes are cleaned daily with IPA or MeOH and
purged with Nj. Syringe Kleen is used to remove metal
deposits in the barrel.
3. Syringes are baked out overnight in the oven of the gas
chromatograph at a minimum temperature of 60''C.
v n . Sample SpUts
If desired, TRC's clients or any party, with the approval of TRC's cUent,
may use sample splits to verify TRC's soil gas or groundwater sampling
results.
A) Sample splits may be coUected in two valve, flow through-type all-glass
or intemally electroplated stainless steel containers for analysis within 10
days of colleaion.
1. Row through sample collection botties should be cleaned by
purging with nitrogen at 100°C for at least 30 minutes. Once clean, the
bottles should be stored filled with nitrogen at ambient pressure.
2. Sample bottles are fiUed by placing them in the sample
stream between the probe and the vacuum pump. Five sample
bottle volumes should be drawn through the container before
the final sample is collected. The sample should be at ambient
pressure.
B) Sample spUts can be provided in 10 cc glass syringes for immediate
analysis in the field by the party requesting the sample splits.
C) Splits of the aqueous standards or the methanol standards used by TRC
for instrument calibration may be analyzed by the party requesting sample
spUts.
1
11
T r a c e r Resea rch C o r p o r a c i o n
Figures 1 through 4
12
i. •
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SY7^///Ga NEEDLE HOSE
C L A M P
RueaET? TUBE
IA< I//. TUB/NG
S-AET.
S / L i e ONE RUS SER W S E CONNECTION
TO VACUU.U PUMP
\. ADAPTER FOR SAMPLMG SOIL -GAS PROi
CLEAR TUB/NG SLEEVE CON//ECTOR (DISPOSABLE)
- S O / L - G A S FLOW OURI//G S A M P U / / G
- 3 X 4 I N . GALVaNIZED PIPE
b < . ^ • O E T A C f / A B L E DRIVE POINT
FIGURE 1. SAMPLING APPARATUS
IA. CLOSE-UP OF SYRINGE SOIL GAS SAMPLING THROUGH EVACUATION LINE IB. DIAGRAM OF SOIL GAS SAMPLING PROBE WITH ADAPTOR FOR
SAMPLING AND EVACUATION OF THE PROBE AFTER IT IS DRIVEN INTO THE GROUND
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I - , • T
—
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— - - L - : I— • • 1 1 : • 1 '
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SITE H.APS TO Iir.OLCTlE: SITE IT^J^E, SCALE, NOF.TH .--TnTiTTOwr; z VJTTU^;^:??: . rryT.Trrair. awn NATL*KA7, F E . - . T T
.%CW, SOIL GAS ; 5 TO IDEi-TIFT
FIGURE 2B EISLS LCGECOK - SITE MJ..?
DATE : ; i - U - 3 ' i . LOCATION : ;?^tD^oi <:Xc/VK-(<- ^ .>-yfr>T7fy)/l/f , 5P CLIENT :. g,c^i?^/^^uAir £ tfv.
GC O p e r a t o r : f. cXc/A5^^ F i e l d A s s i s t a n t : M- AX^€'J?CI^I Weather : /^-;r / ^ « ^ ^c^y^ut ^ Ai^} c SA^e^
F I E L D H O U R S
^ i m e on s i t e BTime off s i t e
i r7 jJ^ /r->o
Hours on s i t e ( B _ A
Lunch hours Downtime hours^ Standbv hours^
) /^
D E C O N T A M 3* iX^'
Probe Decontamination
:otal hours: 7'7
Verified by GC operator
T I 0 K
•^^* Syringe Decontamination
^ » " Total hours : /^
/Tf /^ Ve: r i f i e t i by f i f i e l d a s s i s t a n t
D A I L T S U M M A R Y
Calibration
Time start : ff73^ Time end : <jfj
Total hours: /
Field data and
—
gas
Samoling
Max vacuum : 3 Probes used : / 3 Points used ; yiy> Soil gas samples collected ": /^
Water samoles collected : ^
standards checked
in
by
Hg
Analysis
Total system . blanks : ' Total air samples : J
7/7/ A f ^ ^ ^ Data checking h o u r s : yy '
1
2
Downtime includes time spent repairing sampling & analytic equipment; note times and explanation on following field data pages
Standby includes time available for sampling but waiting for client; . note times and explanation on following field data pages
FIGURE 2C FIELD LOGBOOK - DAILY SUMMARY
O A T c : 2 . ' l i ' j ' f
L O C A T I O N : SA^IO^cf^ i>/eA{fi:XL^ i ,Hy77»4J^, 5 P C L I E . T : SJ.H-'IPG^Jfli/^U. ~A/\i
S A M P L I N G O A T A
T I M E SAMPLE
UJ
c
(u cs 0 tc 0.
< < P
RO
BE
P
U3
II/
PO
UN
D
5
o 2 < Ui > :; Ui —
1-
SA
MP
LE
PO
KIT
S
N O T E S / A O O ' L OATA REQUESTED S r CLI£.'<T
TIHE ON SITE: O 7 j o BEGIN CUIBRATICN: c-yjO
^ ^ ; 2 2 ^ 77:/i.':soi\ M A':SOf\E 7/\
Sho •: j z -o^ : ^ :-7'52 - . i ^ . . ' \3'--3oA^ f '• r . ^ l o a ^ c i <^ iXy4i fA^-iysr n J^AJ>. /V-^^/ *<«^
' • - • ' • '•j^r.i.,,^^ '• '• X ^ ^ ^ ytt^M^if If o<^*A"G> -n i7iA cc^arrewy
" ~ : • : : •..f-rC . • - ^ ^ : ^ : ' • s f f M . , / i ^ i i y,/(ffa> TTicaiM &f<jt.Y-/yzHeo i - f sycn^
<?'// \ Ai-^o ':S/7\^-X0 \ ^ ^ , \ A j a t \ S \ / \ ^'^-^'^'''*^^ * ^ ^ ^ ^ Ai^^^ii^y
^ M M ! M Us^ MM 7cm
\ : i i* L_ .1 1— i \ i—I— . _ —
FIGURE 2D FIELD LGGBCOK - SAMPLING DATA
TRflCER RESEnRCII CORPORnTIOM JOO- onviDSou ci iEnicnL, LnHiiioRN, SOUTH DfiKoin
1 DOTE- 16 FEDRUnRV 1989 CHEMIST- S CIIURDLES
GEOLOGIST- M FnVEROlM
A
DETECTOR n <0 or I> DETECTOR U <Q or 1> RETEMTIOd TIMES SOMPLE ItUECTION <uL>
COMP 1
1 0
0,70 5
COMP 2
1 0
1.1 3
COMP 3
STflMDnRD COMCEHTRnriOM <irc)/L>: — 3^ 10 1 . 3 1 10
3 : »10?19Q 1 215n5?Q 1 1I2637Q
. : 1 1
fi
7
0
SOMPLE
• 1120 DLHIIK H2 DLnilK
n i R SOMPLE
TiMe<n/Q)inj n iru
1 ^ 3 3 000
0 023 SYSTEM DLflMK O 013
SGOl-3' SGOl-3'
HS-ie I S-18
911 917
935 1003
1 2 3 ' ' ^
1000
1000 1000
1000 1000
1 1
B
1 3
fiREn
- 1 0 0 0 -1000
2000 2001)
15312 1790S
3 1 2 1 3650
COHC.
1 4 ERR - 0 . 0 9 7 9 7 - 0 . 0 0 0 1 0
ERR 0 . 0 0 0 9 7 9 0 . 0 0 0 9 7 9
ERR 0 . 0 0 7 5 1 3 0 . 0 0 0 0 1 1
ERR 1 .677301 1 .760099
HEHH
< 0 . 1 < 0 . 0 0 0 5
0 . 0 0 1 0.001
0.000
1 5 2
nREn
-IOOO -1000
-1702 5560
5100 5071
-1000 -IDOO
CONC.
ERR - 0 . 0 0 2 1 5 - 0 . 0 0 0 0 1
ERR 0.0D0Q57 O.OOOUGO
ERR 0.000066 0.000072
ERR -0.01227 - 0 . 0 1 2 2 7
HEOH
< 0 . 0 0 2 <.OOOOl
.00006
.00007
.00007
<0.01
riREO
-1000 -1000
12569 10721
331623 110552
10320 -11715
COHC.
ERR -n.OOQOS - 0 . 0 0 0 0 1
ERR 0 . 0 0 0 5 5 6 0 . 0 0 0 1 7 1
ERR 0.015560 0.010169
ERR 1.793190 1.970706
MEOH
<.009 <.OOOOI
0.0006 0.0005
0.02
2
FiaunE 3 . EXPLnilATIOll OF FIELD DATA SHEET
t. f U * And tt«(( lAf«r»atl«n.
I. CoBCantratloA eC «n«lrt« In calibration ctAndard.
4. faali «ta*t «bk*tit«4 <ro* •tandaid |n)«ctl«A* dutlflg <allbcatloK.
I. fl*ar«ni* (actsr (Rr) far <«i»p«»nd obtainad Iron tKra* «allbratlo« tuna. Tha r n «r* at<d for calculation •( oct««t eoncanttatlena «(i4 arc Inclvdad Oft oacb dak* shavt.
I. Patar bltltk varUlaa f^'^^T of OtAndard «at*r ond cUanllnaaa of iaja<kt04 airatcn.
T. Hltregan blaaK voclllo* d«eont*nlnatloA oC orrlAg** ond analytical o<it>lp.
I. Jlir tanplt gtvti AnbUnt eoAcantrotlono /or conporlten with oirataw b U n k .
lyatan blank v a r l M a * dacontaAlnatlon of aarpltng tqulpxant.
t«P)pla ID fiumhari taoi-S*. (ooll 9«» «a*pLa 1 takan ft* balotf fiada), HS-lt (watar oavpla).
Tloa o( onolyala lilantlflaa tho chccftitogran fro* whlck tho data waa taken.
Amount o( oaopl* Injaction • oaad lor concantfatlon oalculatIen.
raah arao - raw data prediicad hf tka computlnf Intagralor that la proportional to tha «a«a «! analfta 1» tha aaaipla,
Act«4l concantration praaant In tha aa»pla coundad to I alfnltlcant flgjro.
H«*n c^'rontrntLoA e( dspllcnta ln)actlona.
!< : ^ - ; j . iY
IifiTE " e i - 2 7 - x ? TIHE •• ± 5 : 2 6 F I = 1 . FE= 1 . FRE3o 'EHTER' TO xK I F ILE HFiHE=" cWH FlrtE FUNCTION TT= . y i TF^ " ftZ TT= .Q-i TF=" Ff-. 77=
. ' • ! ; ' - ! = i
F EHTR'
VHLUE
TV= i
Length 6, Du.._njL
Wr- !t \C)
Support ihcojrDJti
Carrier G s * Rntsmj~r J in lr.!« Pres 3,<. p-u Rite ' ^ iri'mi.-,
CHART S ? = = D _ J SAMPLc Sae -* 1
QpOTWNffig.'^rOT'gT
Detsctor t:'' •.• Vd?3qe , ? ' ^ ' 'A-Sennt. .
Flo-w RJ'.es, .TMi'min Hydt rT^ A i r _ Sccvs-.ge Soiit _
Columa Initul ' ^ . ' i f i F i n a i _ Rate . .
Solvent Cooci,
HETHOn .HUHEES:nH=
E.MI OF ClflLOG fl7= 22 0F=2e P7=18i'5y
CKfth'HEL K
5c)'c sToiJ^^jj^ IH..IEC7_ e i - 2 7 - 3 5 1 5 : 4 2 : 6 4
fi'z 1
FILE 1.
PERKS
1 2 7
4
6 7
HETHOn
flRE.q;^
e. 277 1.754 e . 164 0 .152
25 . 031 2 6 . 3 5 1 4 5 , 5 2 1
0.
RT
e. 24 Q. 43 8. 35 6. 53 1. ?2 2 . 7 5 6 .26
RUN 1
RREfl EC
12779 02 64134 02 s e n Ql 5547 61
9177S8 61 936147 81
1565623 9 1
V31-27-35 1 5 : 4 3 : 9 4
IHBEX 1
CH= "R" p::.= i .
T07flL 180. ?639014
FIGURE 4 CHROMATOGRAM DOCUMENTATION