3411 SILVERSIDE RD., 10 ILMINGTON, TELEPHONE (302) 478-1522 l FAX (302) 464097 DE 19810 October 27, 1995 Ms. Debbie Lumpkins Office of OTC Drug Evaluation (HFD 812) United States Food and Drug Administration 7520 Standish Place Rockville, MD 20855 Attn: Dockets Management Branch (HFA305) Food and Drug Administration, Room l-23 12420 Parklawn Drive Rockville, MD 20857 Re: Chloroxylenol (PCMX) Handwash Retention Study Dear Ms. Lumpkins: As discussed in my meeting with you and Lee Geismar of 12/l/94, NIPA Hardwicke has been trying to determine a “ball park” figure for the amount of PCMX retained on the skin after a routine five minute handwash. The reason we felt that this information was needed, was to have a reasonableidea of where to begin a dose-rangefinding study which was requested as a prerequisite to FDA’s required 18 month mouse painting study. Your files will show that after FDA’s initial review of our proposed 18 month mouse study protocol, FDA requested a short protocol for the dose-range finding study During our referenced meeting and subsequent discussions, you indicated that you thought the retention evaluation was a reasonablepreliminary step. During that meeting I committed that I would share that handwash retention evaluation with you when completed. Two copies of that evaluation are enclosed for your review. Please expedite your review of the enclosed handwashing study and give us your feedback so that we may have our contractor draft a dose-range finding study for your review.
Ms. Debbie Lumpkins Office of OTC Drug Evaluation (HFD 812) United States Food and Drug Administration 7520 Standish Place Rockville, MD 20855
Attn: Dockets Management Branch (HFA305) Food and Drug Administration, Room l-23 12420 Parklawn Drive Rockville, MD 20857
Re: Chloroxylenol (PCMX) Handwash Retention Study
Dear Ms. Lumpkins:
As discussed in my meeting with you and Lee Geismar of 12/l/94, NIPA Hardwicke has been trying to determine a “ball park” figure for the amount of PCMX retained on the skin after a routine five minute handwash. The reason we felt that this information was needed, was to have a reasonable idea of where to begin a dose-range finding study which was requested as a prerequisite to FDA’s required 18 month mouse painting study. Your files will show that after FDA’s initial review of our proposed 18 month mouse study protocol, FDA requested a short protocol for the dose-range finding study
During our referenced meeting and subsequent discussions, you indicated that you thought the retention evaluation was a reasonable preliminary step. During that meeting I committed that I would share that handwash retention evaluation with you when completed. Two copies of that evaluation are enclosed for your review.
Please expedite your review of the enclosed handwashing study and give us your feedback so that we may have our contractor draft a dose-range finding study for your review.
NIPA Hardwicke is anxious to complete our work on PCMX as soon as possible. Your assistance in and timely response to this matter will be greatly appreciated.
Sincerely,
Irving Gottlieb Director of Sales and Marketing, Biocides
cc: G.R. Kramzar
Dr. W. Guess
Studv Title Determination of PCMX retained on hands after washing with a handsoap containing 3% Nipacide
PCMX (Chloroxylenol). Fii Report.
Author and Analvst Mehdi R Yazdi, PhD.
Studv Comdetion Data This study was started on August 30,1995 and completed on September 28,1995
Performiw Laboratory NIPA Hardwicke, Inc.
2114 Larry Jeffers Road Elgin, S.C. 29045
Proiect ID Number 1221
Records The raw data for this report is recorded in laboratory notebook MRYO28,PP. 023-030; 065-067 and
filing folders. They are also kept in Archives of the performing laboratory
Snonsor
NIPA Hardwicke, Inc. 3411 Silverside Road
104 Hagley Bldg. Wilmington, DE 19810
Page 1 of 37
Statement of Data Confidentiality Claims
Determination ofPCh4X retained on hands after washing with a handsoap containing 3% Nipacide PCMX (Chloroxylenol).. Final report.
Proiect ID Number 1221
No claim of cotidentiality is made for any information contained in this study on the basis of its’ f&g within the scope of the EPA’s Federal Insecticide, Fungicide, and Rodenticide Act (FIFRA) 10(d) (1) (A), (B), and (C), or the FDA’s Federal Food, Drug, and Cosmetic Act (ZFDCA), or any other rules or regulations published by either the EPA or FDA
lBla7h3- Date of Signature
Page2of37
‘ . . ‘, .
8 I ! !
Statement of Laboratory Quality Policy
Quality = “Cox&ormance to the Requirements”
At the analytical services laboratory, we analyze material under tight specifications with implementation of zero defect policy. NIPA Hardwicke Incorporated at Elgin, South Carolina is a manufacturer of Specialty Fine Chemicals and Bulk Pharmaceutical Chemicals. The entire facility is IS0 9002 Registered with Registration No. FM 25491. This facility has been inspected by the FDA, and audited several times by major phamxxeutical companies this year, Neither any obje&ions nor any negative observations have arisen during FDA inspection or customer audits of this laboratory. The performing test laboratory passed favorably through FDA and customers inspections.
Date
Manager, Chemical Research & Quality Control
Mehdi R. Yazdi, PhD 1420 95
Date . NIPA Hardwicke, Inc.
Author dz Analyst
Page 3 of 37
Quality Assurance Statement
Studv Title Determination of PCMX retained on hands &er washing with a handsoap containing 3%
Nipacide PCMX (Chloroxylenol). Final report.
Pro&t ID Number 1221
The Quality Assurance Unit (QAU) has reviewed this report and determined that it accurately describes the methods and procedures used and that the results and conclusions herein accurately and lily reflect the raw data from this study.
All procedures performed during this study are accurately described in the procedure section of this report. Applicable Standard Operating Procedures followed in this study. There were no discrepancies between the procedure and data of the laboratov notebook, filling documents and this report.
The QAU inspected an actual phase of this study and reviewed the laboratory notebook and this report on the dates indicated below.
Study Inspected On: % =J- -qr
Notebook Inspected On: / 0 - 2 d - ?r
Report Inspected On: /&I- Q* 9r
Manager, Chemical Research & Quality Con+
Mehdi R Yazdii PhD. NIPA Hardwicke, Inc.
Author & Analyst
ID- 26 9r Date
Date
Page 4 of 37
Summarv
Study Title Determmation of PCMX retained on the hands after washing with a handsoap containing 3% Nipacide PCMX (Chloroxylenol). Fi report.
An attempt was made to determine the amount of PCMX retained on the skin of hands after washing with a handsoap containing 3% Nipacide PCMX (Chloroxylenol). In order to a thieve this objective, one had to measure the amount of PCMX rinsed off the hands.
Three volunteers washed their hands for five minutes with a handsoap containi@%NipacidePCMX (Chloroxylenol).
Initially hands were rinsed off with 25OOml of deionized water into a stainless steel basin and followed by 5OOml of reagent alcohol into a glass crystaking dish. Samples of the rinsed water and reagent alcohol were analyzed by high perEormance liquid chromatography (HPLC) technique for PCMX content. An average of 89.8% of PCMX was found in the rinsed water and 7.23% in reagent alcohol, with 97% total PCMX recovery.
Page 5 of 37
Studv The Determination ofPCMX retained on hands after washing with a handsoap containing 3% Nipacide PCMX (Chloroxylenol). Fii report
Proiect ID Number 1221
Obiective The objective of this study was to determine the amount of PCMX retained on the skin of hands atIer washing for five minutes with a handsoap formulation conmining 3% Nipacide PCMX. To meet this objective it was necessary to measure the level of PCMX recovered from the water and reagent alcohol rinsates used after the five minute washes.
Materials A handsoap containing 3% Nipacide PCMX (Chloroxylenol) manufactured on 6/30/93 by Huntington Laboratories Incorporation, 9’7OE Tipton Street, Huntington, IN 46750. This soap was analyzed by the soap manufacturer and Nipa Hardwicke Inc. Both analyses showed shniliar results: 2.958% and 2.963% PCMX, respectively.
Deionized water, from Environmental laboratory.
Reagent Alcohol, 90.19% (OMNISOLV, AXO445-1, Lot # 34339).
CMS Disposable Transfer Pipettes (Catalog # 028-795).
F ilter F lasks, 4OOOml with Tubulation, Pyrex
Cry-g Dishes, 1OOOml (CMS # 077693)
Stainless Steel Bowl, 7 Quart (CMS # 039-321)
Pipet F iJler (CMS # 269-654)
Laboratory Clock
StirringBars
Hot Plate/Stirrer, Corning Model PC35 1.
M icrospatula
See Appendii A for mobile phase; the HPLC method for Assay of PCMX and Trial #2 Chromatograms (only one injection of each sequence study was shown).
Procedure
A: System calibration and procedure accuracy (iucluding method and operator):
In order to determine the procedure suitability and integrity of data all the standards were prepared in duplicate, and system calibration and sample analyses were done as following:
&== Standard PCMX in water/calibration “duplicate standard”
Rr = 3% Nipacide soap in water/reference
Page 7 of 37
RZ = 3% PCMX Nipacide soap in water/reference “duplicate reference”
Sr,S& = 3% PCMX Nipacide soap rinsed off from volunteers hands (samples in water)
Bz = Reagent. alcohol/blank
C3 = Standard PCMX in reagent alcohol/calibration
Cd = Standard PCMX in reagent alcohol/calibration “duplicate standard’
&,s&= Nipacide soap rinsed off from volunteers hands (samples in reagent alcohol)
Cl = Standard PCMX in water/ “system petiormance”
B: System suitability for analysis of Nipacide soap in water layer:
0 Procedure and method suitabiity for PCMX recovery in water layer was found to be 99.40%. In a 4OOOm.i filter flask, add 2500ml (by volumetric flask) of deionized water. With a 5ml
serological pipet, add 5ml of a handsoap containing 3% Nipacide PCMX (Chloroxylenol) (with no air bubbles) into the flask.
0 Rinse the pipet 10 times with the solution and stir the solution for 10 minutes with a magnetic bar on a hot plate&irrer. Prepare it in duplicate and analyze both reference samples for assay by the HPLC method.
l In a 25ml volumetric flask weigh O.OSg-O.083g of reagent grade PCMX and dilute it with 1Oml of reagent alcohol. Shake the solution well and add water to the mark. Shake it well again and adjust the volume to the mark with water if necessary.
Page 8 of 37
r
,
l Then pipet 5ml of this solution with a Sml glas s pipet into a 25Oml volumetric flas k and add water to the mark. Shake it well. Prepare it in duplicate and analyze both calibration samples by the HPLC method.
Calculation
Since the purity of reagent grade PCMX is : 99.5% and the content of PCMX in a handsoap containing 3% Nipac ide PCMX (Chlorox y lenol)is : 2.958% , one can obtain the whole s y s tem suitabiity in the water layer by:
Content of PCMX in 3% Nipac ide soap (accuracy and precis ion):
% PCMX = Avg. Smn. area x 99.5% x Avg. Std. wt cm&@ Avg. Std. Area x Smp. wt. (mg/ml)
W hereas:
Avg. Smp. Area: Average of two injec tions peak areas for a sample
Avg. Std. W t. Average of two s tandards weights
Avg. Std. Area: Average of four injec tions peak areas from the two s tandards.
and
% PCMX recovered = Avg. % PCMX found in soan x 100 2.958%
C: System suitability for analy s is of PCMX in reagent alcohol:
l Procedure and method suitabiity for PCMX recovery in reagent alcohol was found to be 99.45% . In a 5Oml voIumetric flas k weigh 0.08-0.083g of reagent grade PCMX and dilute it to the mark with reagent alcohol. Shake it well. W ith a lml glas s pipet, pipet lml of this solution into a 1OOml volumetric flas k and dilute it to the mark with reagent alcohol. Shake it well. Prepare it in duplicate and analyze both calibration samples by the HPLC method.
Page 9 of 37
,I ,I * .
; I I I
Calculation
S tandard vs. S tandard (Accuracy and Precision):
% PCMX =Avn. S tdr area x 995% x S td, wt. (m&ml) Avg. S tdz area x S tdr wt, (mg/ml)
and
% PCh4X recovered = % PCMX Found x 100 99.5%
D: Determ ination of PCMX retained on hands after washing with a handsoap containing 3% Nipacide PCMX (Chloroxylenol)
l This study began by volunteers wetting their hands with tap water. Then they placed their hands over the stainless steel bowl and 5Om l of a was dispensed by serological pipet into their cupped hands (note that the soap contains no air bubbles in the pipet).
l The volunteers spread the soap evenly over the hands and they rubbed their hands thoroughly for 5 m inutes. Each hand rubbed across the cuticles, knuckles, the back of the hands, palms and across on each of the four sides of each finger and between each tinger.
l AtIer 5 m inutes of washing while the hands are still over the bowl, the ass&ant slowly poured deionized water over the hands and the volunteer start to wash off the soap from hands.
l After pouring 1OOOm.l of water, the volunteer rub his/her hands for about lo-20 seconds and another 1OOOml of water poured in into his/her hands while volunteer washing off the soap from hands.
l Again the volunteer rub his/her hands for another 10-20 seconds and SOOml of water poured in slowly into the volunteer hands for final rinse with water. Total of 25OOm l of deionized water was poured into and over the hands and the total volum e was collected in the bowl.
l Then the assistant rinsed the pipet 10 tim es with this solution (25OOm l), in order to assure total sam ple recovery. A stirring bar placed into the bowl and the solution was stirred for 10 m inutes.
l After 10 m inutes of stirring, the pipet was rinsed off again for 5 m ore tim es and the solution in the bowl was swirled for lo-20 seconds (for total PCMX recovery in the water layer purposes).
Page 10 of37
-. G, ’
, t
r’ ,I ‘I
l Then stirred the som tion for another m inute. Then the solution was allowed to stand still for lo-20 m inutes prior to sam pling for analysis.
l After rinsm g hands with 25OOm l water, immediately the volunteer placed his/her hands * over a 1OOOml crystalking dish. 5OOml of reagent alcohol was poured slowly over and into the hands while the volunteer rubbed and washed off the rem aining of PCMX soap f?om his/her hands.
l Once the dispersing of reagent alcohol is finished, the volunteer continued washing and washing each hand for 3 m inutes (to assure total PCMX recovery form hands). A fter total of six m inutes washing and washing, the vohm teer rem oved his/her hands fi-om the dish. Then the crystalking dish solution was swirled for about 30 seconds. This solution, let stood still for 20-30 m inutes prior to sam pling from HPLC analysis.
The above procedure was repeated three tim es with three volunteers on three different days.
Calculation
a: Content of PCMX in water layer:
Determ ination of PCMX in water layer is determ ined by an external standard technique as following:
% PCMX = Avg. S m n. Area x 99.5% x AVB, S td. W t. (mg;/ml’l Avg. S td. Areax S m p. W t. (mg/ml)
Whereas:
Avg. S m p. Area: Average of two injections peak areas for a sam ple
Avg. S td. W t.: Average of two standard weights
Avg. S td. Area: Average of four injections peak arees from the two standards
S m p. W t(m ): m = V x d;,m = 5ml x l.O4g/m l= 5.2g/25OOm l= 2.08m g/m l
Density(d): Found to be 1.04g!m .l
b: Content of PCMX in Reagent Alcohol Layer
Determ ination of PCMX in reagent alcohol layer is obtained by an external standard technique as following:
Page 11 of37
AVE. Smu. Area x Avg. Std. Wt. (ppm) = ppm (PCMX) Avg. Std. Area
Cram 0fPCMX = ppm (PCMX)/lOOO,OOO x 500 ml
c: Total Recovery:
Since the content of PCMX in the soap is X% (average of (RI + R2)/2 value) and since 5ml of 3% Nipacide PCMX soap is used for hands cleaning, therefore, the total PCMX recovered is:
(A) Cram of PCMX used for each volunteer = 5.2g x Xg 10%
(B) Gram of PCMX found in water = % PCMX in water (Part a) x 5.2g
(C) Cram of PCMX found in Reagent Alcohol = Obtained from Part b
Therefore:
(D) % Recovered PCMX in water: (B)/(A) x 100
(E) % Recovered PCMX in Reagent Alcohol: (C)/(A) x 100
% Total Recovery = (D)f (EZ)
Results:
Table I shows the HPLC analyses of rinsed soap containing 3% Nipacide PCMX fkom volunteers hands in the water and reagent alcohol layers. The chromatographic data from this table indicate that over 96% PCh4X recovered for each set of this study with 97.0% overall recovery. Also, fi-om these data and results, it appears that an average of 7.23% PCMX (or 11 .OSmg) was found from a total possible retention of 10% on the skin.
Page 12 of 37
Table I: HPLC ANALYSES OF PCMX IN WATER AND ALCOHOL RINSE
Sample Code
SUP 09/20/95
CAB 09/20/95
CXB 09/20/95
SUP 09/25/95
cm 09/25/95
CHB 09/25/95
SUP 09/27/95
CAB 09/27/95
CHB 09127195
PCMXiIt soap@
0.15275
0.15275
0.15275
0.15314
0.15314
0.153 14
0.15314
0.15314
0.15314
PcMxin PcMxin Water Layer Al#hol
b9 Layer (g) 0.14768 0.00450
0.13884 0.01050
0.13156 0.013%
0.14352 0.00460
0.13572 0.01272
0.133 12 0.01351
0.14% 0.00569
0.12844 0.01730
0.13156 0.016%
Average:
PCMXiII PCMXin TO&l Water (%) AkxW (%) Recovery (%)
%.68 2.95 99.63
90.89 6.87 97.76
as.13 9.14 95.27
93.72 3.00 %.72
88.62 8.31 %.93
86.93 8.82 95.75
95.08 3.71 98.79
83.90 11.30 95.20
85.91 11.01 %.92
89.8% 7.23 97.0%
Page 13 of37
APPENDIXA
Studv Title Determination ofPCMX retained on the hands after washing with a handsoap containin& 3% Nipacide
PCMX (CUoroq4enol).
Final report
Proiect ID Numbers 1221
Page 14 of 37
Method,: C:\HPCHEM\l\METHODS
Method Information
This is a method for analysis of 4-CHLORO-3,5-DIMETHYLPHENOL(PCMX) in (a)as is (b)formulated soap (c)water and (d)reagent alcohol. column: ZORBAX SB-PHENYL,3.0 mm ID X 25Cm with serial number DP-1006. MOBILE PHASE PREPARATION: CHANNEL A: HPLC GRADE ACETONITRILE(OMNISOL, AXO142-1, LOT# 35111). CHANNEL B: IN A 1000 ml ELUANT BOTTLE ADD A LITER OF REAGENT, SOLUTION
DEIONIZED WATER ALDRICH CATALOG FOR 15 MINUTES.
AND 3 DROPS OF 85% PHOSPHORIC ACID(A.C,S. No.21,510-4, LOT# 0222OKX). SONICATE THIS
Run Time Checklist
Pre-Run Cmd/Macro: off
Data Acquisition: on
Standard Data Analysis: on
Customized Data Analysis: off
Save GLP Data: off
Post-Run Cmd/Macro: off
Save Method with Data: off
LC 1090
Pump (DR5) :
Stop Time Post Time Flow Min. Pressure Max. Pressure Oven Temperature
13.00 min 1.00 min
0.500 ml/min 0 bar
400 bar 40.0 Centigrade
HP LC System Thursday, October 19, 1895 12:03:34 PM by JTH3 15 OF 37
Page 1 of 5
I@thod\ C:\HPCHEM\l\METHODS MX.M , I I
Solvent A 50.0 % (ACN) Solvent B 50.0 % (PH=3/H3P04) Solvent C Off
5.000 % 0.000 min 5.000 % 0.000 min 1.000000 (if not set in sample table) 0.000000 (if not set in sample table) not reported no calibration if peaks missing
Curve Type Origin, :
Linear Included
Response Factor Update: Average Response Factors of all calibrations Retention Time Update : Floating Average of Retention Times, New 75%
Calibration Report Options : Printout of recalibrations within a sequence:
Calibration Table after Recalibration Normal Report after Recalibration
If the sequence is done with bracketing: Results of first cycle (ending previous bracket)
Signal 1 : DAD1 A, Sig=280,4 Ref=500,50
HP LC System Thursday, October 19, 1995 12:03:34 PM by JTH3 19 OF 37
Page 5 of 5
Sequen&e: C:\HPCHEM\l\SEQUE I 1 r I
Operator:
Data Subdirectory: Part of Methods to run:
Wait Time after loading Method:
Barcode Reader:
Sequence Timeout: Shutdown Cmd/Macro:
Sequence Comment:
MEHDI
PCMX Runtime Checklist
0.000 min
not available
60.000 min STANDBY '
Seq. Cal. Method Line Line Name
1 PCMX 2 PCMX
Vial Num.
0 1 2 3 4 5 6 7 8 9
10 11 12 13
Sample Name
WATER STDlA/0.065264 STDlB/0.064552 SOAP/2.08/2500 W SOAP/2.08/2500 W SUZI/2.08/2500 W CARL/2.08/2500 W ,, CHUCK2.08/2500 W BLANK/ETOH STDETOH/16.02PPM STDETOH/lG.lOPPM SUZI,'ETOH/500 CARL/ETOH/500 CHUCK/ETOH/500
Sequence Table
From To Inj / Vial Vial Vial
0 13 2 1 1 2
Sample Table
Sample Multiplier ISTD Amount Amount
HP LC System Thursday, October 19, 1995 12:05:24 PM by JTH3 20 OF 37
Page 1 of 3
Skquelike: C:\HPCHEM\l\SEQUE I I 3 I
Seq. Vial Sample Sample Multiplier ISTD Cal. Method Inj/ Line Num. Name Amount Amount Line Name Vial
1 1 1 1 1 1 1 1 1 1 1 1 1 1 2
0 WATER 1 STDlA/0.065264 2 STDlB/0.064552 3 S0AP/2.08/2500 w 4 S0AP/2.08/2500 w 5 suzI/2.08/2500 w 6 cmL/2.08/2500 w 7 CHUCK2.08/2500 w a BLANK/ETOH 9 STDETOH/16.02PPM
Print one page header: Print Configuration: Print sequence/sample table: Print logbook: Print method(s) : Print Analysis reports: Print statistics for Calib. runs: Print statistics for Sample runs: Summary style: Repo'rt sent to printer: Report sent to file: Print report online:
NO NO NO NO NO NO NO NO Sample Summary YES NO NO
Report parameters activated for statistical calculation:
Retention time Emin] Peak area [mAUs or [mVsl Peak height CmAUl or [mVl
Limits are related to standard error
HP LC System Thursday, October 19, 1995 12:05:24 PM by JTH3
22 OF 37
Page 3 of 3
Data File C:\H,PCHEM\l\DATA\ \OOO-0102.D Sample Name: WATER , I ,.I -------------------------- --------------------------==========------ ------=-----------------,,,,,,,,, -------------------_------
Acq. Method : PC!MX.M Acq. Operator : MEHDI
Seq. Line : I Vial : 0
Injection Date : g/25/95 5:13:00 PM Sample Name
Inj : 2 : WATER Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HPCHEM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETHYLPHENOL) . column:
Area Percent Report ==========----==========-------------- --------------==============e===================
Sorted by Signal Calib. Data Modified : ' Friday, September 01, 1995 10:01:53 AM Multiplier 1.000000
Signal 1: DAD1 A, Sig=280,4 Ref=500,50
1 Warnings or Errors :
Warning : Time reference compound(s) not found
---- _-_-_-----_-------_-------------------------------~------------------ -----__---------_-_-____________________------------------------- - *** End of Report ***
HP LC System Monday, September 25, 1995 5:23:03 PM by MEHDI
Acq. Method : PCMX.M Seq. Line : 1 Acq. Operator : MEHDI Vial : 1 Injection Date : g/25/95 S:26:38 PM Inj : 1 Sample Name : STDlA/0.065264 Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HPCHEM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETHYLPHENOL) . column:
UADl A, slg=2W,4 Ket=!XlO,SO ofm=1171xRxTnmn - . D
Area Percent Report =====================================================================
Sorted by Signal Calib. Data Modified : Friday, September 01, 199s 10:01:53 AM Multiplier : 1.000000
Signal 1: DAD1 A, Sig=280,4 Ref=500,50
Peak RT TYPe # [mini
1 --_- I--------- I------- 1 1 4.391 BB
Totals :
1 Warnings or Errors :
Width Area Area Name [mini tmAU*secl % ------ I ---------___ I -------- I -------------- I 0.059 383.03711 100.00 ?
383.03711
HP LC System Monday, September 25, 1995 5:36:41 PM by MEHDI
24 OF 37
Page 1 of 2
Data File C:\HPCHEM\l\DATA\PCMX\OO2-0lOl.D *. a, ' Sample Name: STDlB/0.064552
===Ix:z ~a----------------- -------------------====-==Z====I=f-r==-======================= Acq. Method : PCMX.M Seq. Line : 1 Acq. Operator : MEHDI Vial : 2 Injection Date : g/25/95 5:53:52 PM Inj : 1 Sample Name : STDlB/0.064552 Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HPCHEM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETHYLPHENOL) . column:
: g/25/95 6:21:09 PM Sample Name : SOAP/2.08/2500 W
Inj : 1 Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HPCHEM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETHYLPHENOL) . column:
Acq. Method : PCMX.M Seq. Line : 1 Acq. Operator : MEHDI Vial : 4 Injection Date : g/25/95 6:4,8:28 PM Inj : 1 Sample Name : SOAP/2.08/2500 W Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HPCHEM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETHYLPHENOL) . column:
HP LC System Monday, September 25, 1995 6:58:32 PM by MEHDI Page 1 of 2
D.a,ta File C:\HPCHEM\l\DATA\PCMX\OOS-0lOl.D / j Sample Name: SUZI/2.08/2500 w
,*.d.J.&~m'--,---- -------------=======pIpI I -=Pa=x11=x'I'=P193P3=~========-------- --------=x=s==s Acq. Method :PCMX.M Seq. Line : 1 ' Acq. Operator : MEHDI Vial : 5 Injection Date : 9,'25/95 7:15:47 PM Inj : 1 Sample Name : SUZI/2.08/2500 W Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HP&EM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETHYLPHENOL) . column:
HP LC System Monday, September 25, 1995 7:25:50 PM by MEHDI Page 1 of 2
28 OF 37
D,ata File C:\HPCHEM\l\DATA\PCMX\OO6-01Ol.D Samp Name: CARL/2.08/2500 W
‘, II I* f =fPP=P11~31====13’=t~==~== =====‘=P==P”P113P3J3=======-=-~= 1IPP3eafl=’
Acq. Method :PCMX.M Seq. Line : 1 * Acq. Operator : MEHDI Vial : 6 Injection Date : g/25/95 7:43:05 PM Inj : 1 Sample Name : CARL/2.08/2500 W Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HPCHEM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETHYLPHENOL) . column:
HP LC System Monday, September 25, 1995 7:53:08 PM by MEHDI
29 OF 37
Page 1 of 2
Qata File C:\HPCHEM\l\DATA\ X\OO7-0lOl.D Sam Name: CHUCK2.08/2500 w L -12 8' L '=311P==3===IP11=PPI== X1P=lf~ZP=P='S3==3=====~=- -=PIIP~=I=IP31PPe3Pl=~
Acq. Method :PCMX.M Seq. Line : 1 ' Acq. Operator : MEHDI Vial : 7 Injection Date : g/25/95 8:10:24 PM Inj : 1 Sample Name : CHUCK2.08/2500 W Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HP&EM\l\METHODS\PcMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETTJYLPHENOL) . column: r Llbt - .
HP LC System Monday, September 25, 1995 8:20:28 PM by MEZSDI
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Data Eile C:\HPCHEM\l\DATA\ \008-0101.~ ample Name: BLANK/ETOH i ',,, ,. I -w---- ------f-...,---,-e--w- --'-------'--==I=='===~=========== 133=3==*P11==3=131P3===~====
Acq. Method : PCMX.M Seq. Line : 1 Acq. Operator : MEHDI Vial : 8 Injection Date : 9/25/95 8:37:46 PM Inj : 1 Sample Name : BLANR/ETOH Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HPCHEM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETHYLPHENOL) . column: I1.u
mAU ’ l-
0.75 -
0.5 -
-0.75 i
-1 i 1 4 b b . :
Area Percent Report
Sorted by Signal Calib. Data Modified : * Friday, September 01, 1995 10:01:53 AM Multiplier : 1.000000
Acq. Method :PCMX.M Seq. Line : 1 ' Acq. Operator : MEHDI Vial : 9 injection Date : g/25/95 9:05:09 PM Inj : 1 Sample Name : STDETOH/16.02PPM Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HPCHEM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETHYLPHENOL) . column:
Acq. Method :PCMX.M Seq. Line : 1 ' Acq. Operator : MEHDI Vial : 10 Injection Date : g/25/95 9:32:27 PM Inj : 1 Sample Name : STDETOH/lG.lOPPM Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HPCHEM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETHYLPHENOL) . column:
UAW A, SIg=280,4 iW=5OO,SO Ot L u-1 P . mAu .
17.5 -
f5-,
12.5 -
IO-
7.5 -
5-
2.5
1 4 6 8 min
Sorted by Signal Calib. Data Modified : Friday, September 01, 1995 10:01:53 AM Multiplier : 1.000000
Signal 1: DAD1 A, Sig=280,4 Ref=500,50
Peak RT Wee Width Area Area Name # [min] [minl [mAU*secl
De,ta File C:\HPCHEM\l\DATA\P \Oll-0lOl.D le Name: SUZI/ETOH/500 ( :,I 2' c
P3====1xPPPPe================-== '=13PP==o~1~PP3~3==P=~==========~-==~ Acq. Method :PCMX.M Seq. Line : 1 Acq. Operator : MEHDI Vial : 11 Injection Date : g/25/95 9:59:44 PM Inj : 1 Sample Name : SUZI/ETOH/SOO Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HP&HEM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETHYLPHENOL) . column:
Area Percent Report ================================I=======================================
Sorted by Signal Calib. Data Modified : Multiplier :
Friday, September 01, 1995 10:01:53 AM 1.000000
Signal 1: DAD1 A, Sig=280,4 Ref=500,50
Peak RT Tm?e Width Area Area Name # [mini [min] [mAU*secl
1 --mm 1 4.356 BB 0.079 53.56541 100.00 ?
Totals : 53.56541
1 Warnings or Errors :
HP LC System Monday, September 25, 1995 10:09:47 PM by MEHDI Page 1
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Data File C:\HPCHEM\l\DATA\PCMX\Oi2-0lOl.D Sample Name: CARL/ETOH/500 (. i ‘ "~=,r~el=I-----rrPPP=====~~ ---..-w ;==1~==~~~=3=33=~=~========- -.+‘~='P=I~~P9~~===' Acq. Method : PCMX.M Seq, Line : 1 ' Acq. Operator : MEHDI Vial : 12 Injection Date : g/25/95 10:27:00 PM Inj : 1 Sample Name : CARL/ETOH/SOO Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HPCHEM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETHYLPHENOL) . column:
Injection Date : g/25/95 10:54:17 PM Sample Name : CHUCK/ETOH/500
Inj : 1 Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQVENCE\PCMX.S Analysis Method : C:\HPCHEM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMEZHYLPHENOL) . column:
HP LC System Monday, September 25, 1995 11:04:20 PM by MHHDI Page 1 of 2
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Data File C:\HPCHEM\l\DATA \OOl-02Ol.D S le Name: STDlA/0.065264 a '1,) 8. i c: ==='IPPI=s====33 PP=3=PZ101==3111=P=P====-=============== ====rn===yizac!mxE
Acq. Method :PCMX.M Seq. Line : 2 Acq. Operator : MEHDI Vial : 1 Injection Date : g/25/95 11:21:35 PM Inj : 1 Sample Name : STDlA/0.065264 Inj Volume : 10 ~1
Sequence File : C:\HPCHEM\l\SEQUENCE\PCMX.S Analysis Method : C:\HPCHEM\l\METHODS\PCMX.M this is a method for analysis of PCMX(4-CHLORO-3,5-DIMETHYLPHENOL) . column:
