# MRI.REPORT

A _,.>

__**~_"** _'W""" ._,,-,

__ ., __**~.** __ ,_ .....'


# Consumer Exposure to Paint Stripper Solvents Final Repor1

For U.S. Environmental Protection 

## Agency

EPA Contract No. 68-00-0137 Work Assignment No. 4-06 MRI Project No. 9803-A(06) February 28. 1994



## MIDWEST RESEARC'..;**l~, ,~**  -, ". 

### ffJ: ---.---**I·~ _"~**  __**~-** , • ._.._This document has bE**el~** oreoarec for HIP .r.S Environmenta: F**rurl~ctlon** Aqenc, oroducts does not ')I S''1 Jte AqerH:y E"l!j 1fT E' of Pollution Prevention and T)(I' ,5e )f trade names or COfYln-'e r ( d -r'pn' )f mcommendation fc u:+

This documer : , unntec)n rI':) " I-lOP

# MAl. REPORT

Consumer Exposure to Paint Stripper Solvents Final Report

For U.S. Environmental Protection Agency Technical Program Branch, 7404



## Chemical Management Division OffIce of Pollution Prevention and Toxles 

## Northeast Mall, Room G012 401 M Street, SW Washington, 

## DC 20460

EPA Contract No. 68-00-0137 

## Work Aaalgnment No. 4-06 

## MRI Project No. 9803-A(06) February 28, 1994



## MIDWESTRESEARCH INSTITUTE 425 Volker Boulevard, KansasCity, MO64110-2299 • (816) 753--7600 

# I

## PREFACE The objective of this project is to detennine consumer exposures to solvents contained in chemical paint stripping products that have been fonnulated to reduce or eliminate me1hytene chloride content. This report details the results of 15 experimental runs conducted in the Air Consumer Exposure (ACE) Laboratory at Midwest Research Institute (MAt) to measure airborne exposures to solvents dUring the application of commercially available paint strippers. This project was prepared for the Environmental Protection Agency (EPA), Office of Pollution Prevention and Toxics 

### (Oppn, Chemical Management Division, Technical Programs Branch under EPA Contract No. 68-00-0137, Work Assignment No. 4-06. The EPA Project Officer was Ms. Janet Remmers. Dr. Gordon Cash served as the EPA Work Assignment Manager. This report was prepared by Mr. James McHugh, MRI Work Assignment Leader. The MRI Program Manager was Mr. Paul Constant. Dr. George Scheil, Mr. Scott Klamm, and Mr. William C. Bailey assisted with the ACE laboratory experiments. Mr. Jack Balsinger served as the Senior Quality Assurance Officer. MIDWEST RESEARCH INSTITUTE 

# I

Approved:

# ~;[(~ Program Manager

Jack Balsinger Senior Quality Assurance Officer
February 28, 1994

MRI-0Pf'1iR06-01.FFl 

### ()""-.MJ

. 

# )7"';

LlHnHJ:S 

### M. McHugh, CIH ior Industrial Hygienist



### iii

### CONTENTS 

### Preface iii 

## list of Tables vi 1. Introduction

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 1 2. Product Selection 3 2.1 Shelf survey 3 2.2 Productselection.

. . . . . . . . . . . . . . . . . . . . . .. 3 2.3 Product testing 4 

### 3. MRI ACE laboratory Facilities

.. . . . . . . . . . . . . . . . . . . . . .. 5 3.1 Temperature measurements and controls 6 3.2 Relative humiditymeasurements and controls.

.. 6 3.3 Barometric pressuremeasurements 8 3.4 Air change rate measurements and controls 8 3.5 Air mixing 9 4. Experimental Procedures.

. . . . . . . . . . . . . . . . . . . . . . . . . .. 11 4.1 Test protocol " 11 4.2 Preparation of the test chamber 12 4.3 Sampling equipment 12 4.4 Productapplication method 13 5. Air Sampling Procedures " 19 5.1 Nearly real-time air samples " 19 5.2 Integrated air samples 19 6. Analytical Methods 23 6.1 MIDAC Fourier transform infrared analyzer 23 6.2 Integrated air samples .,. . . . . . . . . . . . . . . . .. 25 7. Results and Discussion . . . . . . . . . . . . . . . . . . . " 27 7.1 Integrated air samples 27 7.2 Nearty real-time airsamples.

. . . . . . . . . . . . . .. 36 7.3 Quality control samples 37 7.4 Quality assurance activities 37 8. Conclusions.

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 39 9. References

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 41 Appendices: A. Limited shelf survey of paint stripping products in the Kansas City metropolitan area A-1 B. Operating procedures for the MIDAC FTIR closed cell system B-1 C. Analytical methods C-1 D. FTIR results-air concentrations vs. time 0-1

MRI-OPPi\R06-01.FR V 

# I

### LIST OF TABLES


### Table Page 

### 1 Test chamberenvironmental conditions 7 2 Duration of test runs

.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 16 3 Quantities of product applied and residue removed . . . . . . . . . . . .

.. 18 4 Air sampling and analytical methods . . . . . . . . . . . . . . . . . . . . . . .

.. 20 

### 5 Concentrations of 

### standards 

### 24 6 Integrated air sampling results-Bix Stripper . . . . . . . . . . . . . . . . .

.. 28 7 Integrated air sampling results-Bix Spray-On Stripper 29 

### 8 Integrated air sampling results-Strypeeze

..... . . . . . . . . . . . . . .. 30 9 Integratedair sampling 

### results-Wood Finishers 

### Pride 31 10 Integrated air sampling results-3M Safest Stripper . . . . . . . . . . . . " 32 11 Occupational exposure limits

.. . . . . . . . . . . . . . . . . . . . . . . . . . . .. 33 12 Blind spiked 

### sample results

.. . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 38 

# I

vii

### SECTION 1 INTRODUCTION
The Toxic Substances Control Act (TSCA) mandates the assessment of risks associated with the manufacture and use of new and existing chemicals. In 1985, the Interagency Committee of IndoorAir Quality called for an effort directed at developing an understanding of the magnitude of human exposure to indoor air pollutants, the contributions of various energy conservation measures. and the impact of introducing new consumer products and bUilding materials. As part of this effort, exposure to chemical releases under various conditions from consumer products and building materials in indoorenvironments must be assessed. Chemical paint strippers used by consumers have primarily contained methylene chloride (dichloromethane). Because of concerns about the toxicity of methylene chloride, new paint stripperformulations have been developed that eliminated this chemical or significantly reduced its content. However, there is concern about the toxicity of these new fonnulations. The Office of Pollution Prevention and Toxies (OPPT) received a referral from the Consumer Product Safety Commission about one such substitute, N-methyl pyrrolidone (NMP). The OPPT RM1 process has determined that there is a reasonable basis for the concern about the use of NMP in paint strippers; however, other new formulations may also pose some degree of risk. The paint-stripping solvents selected for this study represent the largest share of the market. They are:

• Methylene chloride (dichloromethane)
• Toluene
• Acetone
• Methanol
• N-Methyl pyrrolidone (NMP)
• Dibasic esters (e.g., dimethyl glutarate. dimethyl adipate, dimethyl succinate) The objective of this study is to determine consumer exposure to solvents contained in commercially available paint strippers under typical product-use scenarios. The products that were tested are those that have been formulated to reduce the content of methylene chloride.

Mf:ll·OPPl\R06·01.FR 

# ,

### Each of the selected products was tested in triplicate under controlled environmental conditions inside MAl's Air Consumer Exposure (ACE) Laboratory exposure chamber for a total of 15 experiments. The paint strippers were used according to the manufacturers' instructions printed on the label. Product application procedures were consistent with previous laboratory studies of methylene chloride paint strippers conducted at the Lawrence Berkeley Laboratory (Girman and Hodgson, 1986).



### 2

### SECTION 2 PRODUCT SELECTION


### 2.1 SHELF SURVEY 

### A shelf survey was conducted at retail stores in the Kansas City, Missouri, metropolitan area to compile a list of chemical paint stripping products available to consumers (Appendix A). Ten retail stores were surveyed, which included home improvement, paint, and hardware stores. A total of 38 paint stripping products distributed by 19 manufacturers were found on the store shelves. The product contents were detennined from the label and from the material safety data sheet requested from the manufacturers. Thirty-five of the products contained one or more of the target compounds. None of the products contained dimethyl succinate. A total of 29 products contained methylene chloride. Of these, only one product contatned methylene chloride as the sole active ingredient. Twenty-eight products contained other active ingredients in addition to methylene chloride. 

### Of these, 27 contained methanol, 14 contained toluene, and 8 contained acetone. A total of 23 products contained ingredients other than the target compounds selected for this study. Some of the product fonnulations included: xylene, ethanol, lsobutane, petroleum distiltants, minerals spirits, stoddard solvent, monochlorotoluene, ethylene glycol, monobutyl ether, glycol ethers, sodium carbonate, calcium hydroxide, and ammonia. Of the products that did not contain methylene chloride, two contained a mixture of volatile organic compounds (i.e., methanol, toluene, and acetone), two contained a mixture of dibasic esters, and one contained NMP.


### 2.2 PRODUCT SELECTION 

### From the list of available paint strippers on the market, the following five products were selected by the MRI Work Assignment Leader (WAL) and approved by the EPA Work Assignment Manager (WAM):

MRI-OPPT\R08-01.FR 

### 3

### • SIX Stripper, Six Manufacturing Co., Inc., Ashland City, TN • BIX Spray-on Stripper, Bix Manufacturing Co., Inc., Ashland City, TN
• Strypeeze, Savogran, Norwood, MA • Wood Finisher's Pride, Creative Technologies Group, GreensviJIe, SC • 3M Safest Stripper, 3M Corporation, St. Paul, MN Each of the selected products was found on the shelves of at least two retailers and contained one or more of the target compounds. A total of nine products met the selection criteria, however, only five were selected due to cost considerations. The fonnulations of the four products that were eliminated were similar to those selected. All of the paint strippers are applied to the substrate with a brush, except for BIX Spray-on Stripper. This product was specifically selected for this study because of its unique application method. Two of the five selected products contained methylene chloride fonnulated with other volatile organic compounds. Strypeeze contained a mixture of methylene chloride, methanol, acetone, and toluene. SIX Spray-On Stripper contained a mixture of methylene chloride and methanol. The fonnulations of these two products are similar to 25 products included in the shelf survey (i.e., products containing methylene chloride and one or more volatile organic compounds). One of the product selected contained a mixture of organic compounds other than methylene chloride. BIX Stripper, which contained a mixture of methanol, acetone, and toluene, is similar to two other products included in the shelf survey. Two of the five setected products contained semi-volatile compounds. Wood Finisher's Pride was the only product found in 

### the shelf surveythat contained NMP as active ingredient. 3M Safest Stripper, which contained a mixture of dibasic esters, was also chosen for the study. One other products included in the shelf survey have a similarformulation.


### 2.3 PRODUCTTESTING Each of the selected products were analyzed by gas chromatography! mass spectrometry (GS/MS) to confirm the presence of the target compounds. The target volatile organic compounds of each of the selected products were analyzed using EPA Method 8260A, Volatile Organic Compounds by GC!MSCapillary Column Technique. The target semivolatile compounds were analyzed using EPA Method 8270A, Semivolatile Organic Compounds by GC/MS-Capillary Column Technique. The presence of all of the target compounds listed on the product labels were confirmed by the GC/MS 

### analyses. 'if**,~i**



### 4 MRI·0PFl'\R08-0',FR

### SEcnoN3 MRI ACE LABORATORY FACILITIES
This studywas conducted in a room-size test chamber located in MAl's ACE Laboratory (room no. 

### 214/216-E). The volume of the test chamber is 1,261

# ns (floor dimension of 14 x 

### 11.4 ft with a ceiling height of 7.9 

### ft). The test chamber is equipped with temperature, humidity, and ventilation controls required to conduct consumer exposure studies under stable conditions. Real-time temperature, humidity, and barometric pressure measurements were collected at 1-min intervals dUring all experimental test runs using WEATHERtronics sensors mounted inskte the test chamber. A Compaq portable computer recorded the temperature, humidity, and barometric pressure data, together with the clock time, onto an internal hard disk drive. A dot-matrix printer printed the data in real time. The following instruments were used for measurements of environmental conditions inside the test chamber:

• MIDAC Fourier-transform infrared analyzer

• MAl-built analog-to-digital converter based on Wintek micro control system module with 12-bit resolution and RS-232 host computer interface

• Compaq portable computer with GWBASIC logging program

• Dot-matrix printer to record all logger operations

• WEATHERtronics SG-21 hydrothermograph

• WEATHERtronics 7105-A analog output barometer

• WEATHERtronics 5120-8 portable humidity probe

• Thermocouples (type K) with Omega TAC 80 thennocouple-to-millivolt converters



### 5

### 3.1 TEMPERATURE MEASUREMENTS AND CONTROLS The temperature within the ACE Laboratory was monitored using two thermocouples connected to an Omega TAC 80 thermocouple amplifier and Iinearizer. The temperature probes were located on the east wall of the test chamber. The temperature was set between 75° and 

### nOF and controlled within ±1.5°F. The temperature in the ACE Laboratory was controlled with dual thermostats using a dedicated air-conditioning unit. The accuracy of the Omega**thermocouple~to~millivolt** 

### converter is listed by the manufacturer as ±7.2° over its entire operating range of 4° to 1832°F. The output of the instrument is listed as 1 mY/OF. The temperature probe was**cali~** 

### brated over a much narrower operating range (32° to 212°F) using ice water and boiling water to achieve an accuracy of ±1

### OF. The temperature measuring equipment was checked prior to each run against a mercury thermometer. The mercury thermometer was checked against a set of certified thermometers (No. 9848), which are traceable to the National Institute of Standards and Technology (NIST). Table 1 summarizes the average. maximum. and minimum temperatures that were measured inside the test chamber during each experimental run.
3.2 RELATIVE HUMIOtTY MEASUREMENTS AND CONTROLS The relative humidity within the test chamber was measured at 1-min intervals using a WEATHERtronics**5120~B** 

### portable humidity probe located on the east wall of the test chamber. The relative humidity was set at a level between 55% and 65% and controlled within ±10%. The humidity in the test chamberwas regulated by a dedicated**air~conditioning** 

### unit, which dehumidifies the supply air entering the test chamber. Due to the low volume of air entering the chamber. control of the humidity within the chamber was limited. The relative humidity within the chambertended to increase when the person performing the paint stripping operation entered the room. No attempt was made to dehumidify the air once it 

### entered the test chamber. The accuracy of the WEATHERtronics humidity probe is listed by the manufacturer as 

### ±2% in the operating range of 0% to 80% relative humidity. The instrument was tested and fully calibrated at the factory. The humidity probe was calibrated at a low humidity point of 12% inside a glass container using a saturated salt solution of lithium chloride in water, and a high humidity point of 75% using a saturated salt solution of sodium chloride in water. Calibration of the humidity recording equipment was conducted once, immediately prior to the ACE Laboratory experimental runs.


### 6

### ...., MRI-oPPnR06-01 

### Table 1. TEST CHAMBER ENVIRONMENTAL CONDITIONS**r.~**

## !til .-•••

;.::-> )"}':'.- r, . _. ________ 

### 1 0.76 76.6 77.2 76.1 59.2 64.4 55.1 

## 2 0.62 76.8 77.5 76.3 56.8 62.9 54.3 3 

### 0.61 76.6 77.2 76.1 61.4 63.9 58.0 

### 4 0.57 75.9 76.7 75.1 60.2 65.6 57.9 5 0.57 75.8 76.6 75.3 60.0 65.1 57.6 6 

### 0.58 76.2 77.0 75.5 

### 56.1 58.9 54.3 7 0.56 75.8 76.6 75.0 60.6 66.8 58.0 8 0.54 76.7 77.3 75.9 57.9 64.7 54.7 9 0.55 76.3 77.0 75.2 59.3 62.2 

### 56.1 10 0.56 76.5 77.5 75.9 61.9 65.5 56.0 

### 11 0.54 75.9 76.8 75.3 65.4 69.6 57.3 

### 12 0.57 76.6 77.5 76.0 62.7 68.2 55.3 13 0.55 76.6 77.4 76.0 55.9 67.7 46.3 

### 14 0.54 76.1 76.9 75.6 56.6 70.2 47.8 15 0.54 75.8 76.6 75.1 54.6 63.8 46.2

### The humidity recording equipment was checked against a wet bulb/dry bulb psychrometer prior to each experimental run. The thermometers in this unit were checked against NIST traceable thermometers. Table 1 summarizes the average relative humidity measured inside the test chamber during each experimental run. The maximum and minimum relative humidities that were recorded dUring each experimental run are also presented.


### 3.3 BAROMETRIC PRESSURE MEASUREMENTS 

### The barometric pressure was monitored using a WEATHERtronics 7105·A analog output barometer located on the east wall of the test chamber. The barometric pressure was not controlled. The accuracy of the WEATHERtronics analog output barometer is listed by the manufacturer as ±O.08% over an operating range of 17.72 to 32.48 in Hg including hysteresis, thermal shift, and nonlinearity. Each sensor was tested by the manufacturer inside a pressurized chamber and compared to an NISTtraceable standard. Calibration adjustments to this sensor are not possible. The barometerwas checked against a mercury Fortin-type barometer. This instrument check was conducted once immediately prior to the first experimental run.


### 3.4 AIR CHANGE RATE MEASUREMENTS AND CONTROLS 

### Air change rates within the test chamber were controlled for all experimental runs. Air was exhausted from 

### the test chamber using a General Metal Works (GMW) vacuum pump controlled with a critical orifice. The critical orifice was sized to achieve an air change rate (ACH) of approximately 0.5 per hour within the test chamber. Air change rates were estimated for each experimental run by measuring tracer-gas decays. Immediately prior to an experiment, the sulfur hexafluoride (SFe ) 

### tracer gas was uniformly mixed in the test chamber by injecting pure gas with a syringe. A sample of test chamber air was continuously drawn from the breathing zone of the worker and measured with the MIDAC Model 2400 Fourier transform infrared (FTIR) spectrometer at 4-min intervals. A decay curve, Ct

# =Co e-AI, 

### was fitted to the SF6 

### air concentration data collected at regular intervals after injection of SF6 

### gas was stopped and the source removed from the test chamber. The parameterestimates, COl the SF6 

### concentration at time t 

### = 

### 0, and A, the air change rate, were estimated by linear


### 8 MRI-OPPl\R06-01

### regression of the log-transformed SF6 

### concentrations VS. 

### time. The SFa

### concentration at time t 

### = 0, 

### Co. and the air change rate, A, were both estimated simUltaneously by least-squares method. The air change rate during each experimental run is presented in Table 1.


### 3.5 AIR MIXING 

### Air mixing characteristics of the ACE Laboratory test chamber were investigated using tracer gas decays as part of EPA-OPPT, Work Assignment 03 (McHugh and Bauer, 1992). The study found that adequate air mixing in the chamber is achieved using two commercially available box fans positioned at two adjacent comers along the long wall. Each fan was mounted on a tubular stand, which positioned the fans to a 30-degree tilt from the vertical at a height of 32 in from the floor. The fan speed was adjusted to 800 rpm.

9

### 11 

### SEcnON4 EXPERIMENTAL PROCEDURES
4.1 TEST PROTOCOL Each of the selected products was tested in triplicate undercontrolled environmental conditions inside MAl's Air Consumer Exposure (ACE) Laboratory exposure chamberfor a total of 15 experiments. The paint strippers were used according to the manufacturers' instNetions printed on the label. The application procedure was consistent

### with previous laboratory studies conducted at the Lawrence Berkeley Laboratory (Girman and Hodgson, 1986). The substrate selected for paint removal consisted of a plywood panel (8

## ff with dimensions of 2 x 4 ft) 

### painted on one side with a primer coat and two finish coats of an oil-base enamel (white). This is the same substrate as that used for a previous study of methylene chloride exposure from controlled use of a paint remover in residences that was sponsored by the U.S. Consumer Product Safety Commission (Girman and Hodgson, 1987). The ventilation rate within the test chamberwas set at approximately 0.5 air changes per hour (ACH). The selected air change rate was one of the two ventilation rates used in the Lawrence Berkeley Laboratory study of methylene chloride paint stripper. The selected ACH represents the ventilation rate in an enclosed room (no open doors or windows) in a typical residence. The performance of a paint-stripping operation in such an enclosed room approximated the "woret-case' scenario. The ventilation rate was measured using a tracer-gas decay method. Airborne concentrations of paint stripper solvents were measured dUring actual paint stripping operations using two sampling methods-integrated air sampling onto solid sorbent tubes for subsequent analysis, and nearly real-time air concentration measurements using the MIDAC FTIR spectrometer. The air sampling procedures are detailed in Section 5.

MRH)PPT\R06-01

### 4.2 PREPARAnON OF THE TEST CHAMBER The following procedures were performed prior to each experimental run to prepare the environment controls and sensors: • The vacuum exhaust pump was tumed on to maintain the appropriate air change rate within the test chamber. • The temperature sensors in the test chamber were checked against a NISTtraceable thermometer. • The temperature within the chamber was adjusted to between 750 

### and 77°F. • The WEATHERtronics 5120-8 humidity sensor in the chamberwas checked against a psychrometerwith the wet/dry-bulb thermometers traceable to NIST. • The relative humidity within the chamber was adjusted to between 55% and 65%. The test chamber was equipped with the following items:

• Product container • 1-qt can

• 7.6-cm-wide brush

• 7.6-cm-wide scraper

• Cheese cloths • Thin polyethylene plastic sheet • Plywood panel (8

## fr! with dimensions of 2 x 

### 4 ft) 

### painted on one side with a primer coat and two finish coats of an oil-base enamel

• Support stand for the plywood panel

• Fisher Scientific balance (Model No. 2-116), capable of weighing up to 5 kg


### 4.3 SAMPLING EQUIPMENT A MIDAC Model 2400 FTIR spectrometer was set up on a benchtop in the instrument room adjacent to the test chamber. The instrument was equipped with a White cell with a fixed path length of 20 m. A flexible, 12-ft Teflon sampling line from inside the test chamber was routed through the wall of the 12 MRI·QPPTlR06-01

### chamber and attached to the inlet of the White cell. A Gast vacuum pump (Model No. MAA-V109-MB) was attached to the outlet of the White cell with a short length of Tygon tubing. The vacuum pumped 

### putted air from 

### the test chamberthrough the cell at a constant rate. The air exhausted from the White cell was directed back into the test chamber using Teflon tUbing. A valve attached to the outlet of the White cell was used to adjust the vacuum within the White cell to less than 2 in 

### Hg. During all experimental runs, the inlet of the Teflon sampling line to the White cell was attached to the breathing zone of the person performing the stripping operation inside the test chamber. Stationary air samplers were 

### positioned at three locations within the test chamber. The airsampters consisted of a battery-operated pump that pulled air at a constant rate through an activated charcoal tube. Sampling inlets were placed at breathing zone height on both the sides of the plywood panel at a centerline distance of 3 ft. The sampler located nearest to the exhaust outlet of the test chamber was designated as the "outlet·1 

### sampler. The one nearest the air inlet to the chamberwas designated as the 'Iinlet" sampler. An additional stationary samplerwas positioned at breathing height in the center of the test chamber, immediately adjacent to the plywood panel. The supply air to the test chamberwas sampled during each experimental run by placing a stationary air samplerwithin the air stream. When the paint stripper contained methanol, a second set of samplers equipped with a silica gel sorbent tube was placed at each location. The stationary samplers were turned on immediately priorto the start of the paint stripping operation. The lIinletll 

### and "outlet" samplers inside the test chamber were turned off and removed from the test chamber when the test subject left the chamber at the end of the paint stripping and cleanup operations. The samplers positioned at the center of the chamber and in the supply air of the chamber were run for an 8-h period. A built-in timer shut off the samplers automatically at the end of the sampling period. In addition to the stationary sampler, a portable, battery-operated air samplerwas attached to the person performing the stripping operation. The sampling inlet was positioned in their breathing zone. The personal air sampler was started immediately prior to the start of the paint stripping operation and turned off when the test subject left the chamber.


### 4.4 PRODUCT APPLICATION METHOD The paint strippers were used according to the manufacturers' instructions on the container label. The application of the paint removers was similar to that detailed in a study conducted at the Lawrence Berkeley Laboratory (Girman and Hodgson, 1986).

MRI-QPPM06-01 

### 13

### Priorto each experimental run, polyethylene 

### plastic sheets were placed on the floor of the test chamber

### and beneath the support stand to collect the paint scraping. The plywood 

### p8fl8I was 

### ptaced on 

### the support stand which poaitioned the panel at a 

### 45-degree angle. The product container, 

### 1-qt can, brush, scraper, cloths, and plastic sheet were individually weighed on Fisher-Scientific balance (Model 

### No. 2-116). The procedure was as follows:

• Each product was shaken or stirred as recommended by the manufacturer and transferred to a 1-qtmetal can. Forthe BIX Spray.()n Stripper, a portion of the stripperwas transferred to the sprayerthat was supplied with the product. • The can and the application brush (or sprayer) were weighed on the balance and the weight recorded on data sheet.

• Thick coats of the product were applied to one-quarter of the panel with a 7.6-cm-wide brush (or with a sprayer).

• The can and the brush (or sprayer) were weighed again on the balance and the weight recorded.

• After the product remained undisturbed on the first quarter section for 10 min, the product was applied to the second quarter using the same technique as described above.

• Afterthe stripperwas in contact 

### with the paint for 15 min (longerfor some products), the softened paint was scraped from the first quarter with a 7.6-cm-wide scraper. The scrapings were transferred to a polyethylene sheet.

• The above sequence was repeated until each quarter of the panel had been stripped twice.

• During the periods between application of the product or scraping of the softened paint, the test subject sat on a stool approximately 1 m from the substrate. • At the conclusion of the final scraping, the substrate was wiped with clean cheese cloths. • The used metal can, brush, scrapper, and cloths were weighed on the balance and the weights recorded.

• The polyethylene sheets that contained the paint scrapings were gathered, folded, and weighed on the balance. The weights were recorded.


### 14 MRI·0PPTIFI06-01

### • All containers, tools, and the folded plastic sheets were placed into a plastic bag and sealed. • At the comptetion of 

### the paint stripping operation and cleanup, two of the three air samplers were removed from the chamber when the test subject left the chamber. The remaining sampler in the test chambers ran for an 8-h duration. The duration of each experimental run is presented in Table 2. The paint stripper was allowed to remain in contact with the paint for the minimum time recommended on the label. SIX Stripper, SIX Spray-Qn Stripper, and Strypeeze were in contact with the paint for 15 min before scrapping. Wood Finisher's Pride and 3M Safest Stripper were in contact with the paint for 30 and 60 min, respectively. Table 2 also presents the durations of time that the test subject spent inside the chamber. The time spent inside the chamber for experimental run nos. 1 through 9 was approXimately 1"Y.z h. The duration of exposure for run nos. 10 through 12 was approximately 2 h because the stripper was required to be in contact with the paint for 30 min priorto scrapping. The duration of exposure for run nos. 13 through 15 was approximately 2 h due to a 60-min contact time required for the strippers. Table 3 presents the amount of the product 

### applied during each experimental run and the amount of residue scraped off the plywood panel. The residue consisted of the removed paint and that portion of the paint stripper that did not volatilize during the stripping operation.

MRI-oPP'NlO8-01 

### 15

### Table 2. DURATION OF TEST RUNS


### &IX Date 

### 07127193 07129193 

### Entered Chamber 14:50 13:48 

### Start Time 14:55 13:53 

### Stop Time 16:25 15:24 

### Exited Chamber 16:40 15:38 

### Duration 

### ofStripping Operation (hr:min) 01:30 01:30 01:31 

### Duration 

### Subject Inside

Test Chamber hr:min 01:50 01:50 01:50



### 16 

### &IX 

# -on S r Date Entered Chamber Start Time Stop Time Exited Chamber Duration of Stripping

Operation (hr:min) Duration Subject Inside

Test Chamber hr:min



# s • Date Entered Chamber Start Time Stop Time Exited Chamber Duration of Stripping

Operation (hr:min) Duration Subject Inside

Test Chamber hr:min 01:25 01:39

01:25 01:45 01:25 01:36

01:31 01:48 01:25 01:36



### 08127/93

10:44 10:55 12:25 12:41 01:30 01:57

MAl-oPP1\R06-01

### Table 2 (Continued)


### Wood F

........ 

## Prt. Date 

### 09101193 

### 09103193 Entered Chamber 12:47 12:47 StartTime 12:43 12:55 Stop Time 14:35 14:48 Exited Chamber 14:55 15:05 Duration 

### ofStripping

Operation (hr:min) 01:47 

### 01:52 01:53 Duration Subject Inside

Test Chamber hr:min 02:05 02:08 

### 02:18

3M 

### Sllreat StrI Date Entered Chamber StartTime Stop Time Exited Chamber Duration 

### ofStripping

Operation (hr:min) Duration 

### SUbject Inside

Test Chamber hr:min

MAI-OPPl\R06-01 

### 09108193 13:37 13:42 16:21 16:40 

### 02:39 02:40 

### 03:03 02:53 02:40 03:03

17

### Table 3. QUANTmES OF PRODUCT APPLIED AND RESIDUE REMOVED

SIX Stripper 

## 1 664 

## 574 2 724 635 3 

## 703 662 Average 

## 697 624 SIX Spray-on Stripper 

### 4 

## 537 408 

## 5 497 484 

## 6 586 

## 450 Averaae 

## 540 447 Strypeeze 

## 7 724 808 

## 8 676 710 9 

## 765 800 Average 

## 722 773 Wood Finishers' Pride 

### 10 

## 884 1104 11 805 1125 12 908 

## 1124 Average 866 

## 1118 3M Safest Stripper 

### 13 

## 837 778 14 775 669 

## 15 786 761 Average 

### 799 

## 736

18

### 19 SECTION 5 

### AIR SAMPLING 

### PROCEDURES
Airborne concentrations of the paint stripper solvents were measured in the test chamber during paint stripping procedures by collecting both nearly realtime and integrated air samples.


### 5.1 HEARLV REAL-TIME AIR SAMPLES 

### Airborne concentrations of the paint stripper solvents and the tracer gas were measured in nearly real-time at the breathing zone of the paint stripper applicator using a MIDAC Model 2400 Fourier transform infrared (FTIR) spectrometer. The instrument was equipped with a closed-path White cell with a path length of 20 m. Air from the breathing zone of the product user was drawn to the White cell with a sampling pump via Teflon tUbing. Repetitive highresolution spectra were averaged every 4 min over the range of 400 to 4,000 em:' with resolution of 0.5 em". Operating procedures for the MIDAC FTIR closed-cell system are detailed in Appendix B.


### 5.2 INTEGRATED AIR SAMPLES 

### Integrated air samples were collected by drawing air through activated charcoal and/or silica gel sorbent tubes with battery-operated, constant-flow samplers. The air sampling methods used for this study are present in Table 4. When available, sampling was conducted according to National Institute of Occupational Safety and Health (NIOSH) standard methods. NIOSH-approved methods were not available for N-methyl-2-pyrrolidone or for the dibasic esters (dimethyl adipate and dimethyl glutarate). A GAF Chemical Corp. method, which is currently used by OSHA, was used for N-methyl pyrrolidone. The dibasic esters were sampled using a Du Pont-developed method. Two air sampling devices were used for this study; the Ametek Model Alpha 2 constant-flow sampler and the Gilian Model HFS 113 sampling system operated in the low-flow constant pressure mode. The Ametek Alpha 2 is a personal air-sampling instrument that moves a constant volume airflow through an external collection device (e.g., charcoal or silica gel tube). An

MRI·OPPnR06-01I\) 

### o Table 6. AIR SAMPUNG AND ANALYTICAL METHODS

Methylene chloride 

# I NfOSH 

# IActivated charcoal

# I0.01 

### to 0.2 Umin 

# IGaschromatography, FlO 0.01 mg per 1005 sorbent

### tube sample 

### Acetone 

### I NIOSH 

### Activated charcoal 0.01 

### to 0.2 

### Umin Gas chromatography, FlO 0.02 mg per 

### 1300 sorbent tube sample 

### Toluene 

### I NIOSH 

### Activated charcoal 0.01 

### to 0.2 

### Umin Gas chromatography, FlO 0.01 

### mg per 

### 1501 soment

### tube sample Methanol 

### I NIOSH Silica 

### gel sorbsnt 0.02 

### to 0.2 

### Umin Gas chromatography, FlO 0.01 mg 

### per 2000 

### tube sample Dibasic esters 

## I Du Pont 

## I Activated charcoal 0.01 

### to 0.2 

### Umin Gas chromatography, FlO 0.01 mg per sorbent tube sample N--Methyl 

# I GAFf Activated charcoal 0.01 to 0.2 Umin Gas chromatography, FlO 0.01 mg 

### per pyrrolidone OSHA 

### sorbent tube sample

MRK>PPl\R06-()1

### automatic flow control system maintains the rate within ±50/0 over pressure drop changes up to 25 in H2

### 0 . The sampler features two tight--emitting diodes that indicate constant flow and battery charge. The Gilian sampling system consisted of a Gitian air sampler attached to the Gilian triple variable-flow sampling manifotd. The universal sampling manifold allowed one sampling pump to collect up to three sorbent-tube samples simultaneously. The airflow through each sorbent tube was controlled individually with separate needle valves. Both the Ametek and GUian sampJing pumps were calibrated before and after each use with a Gilibrator primary flow calibrator (GUian Instrument Corp). The Gilibrator calibration system is based on the thin-film volumetric method, a primary calibration procedure. The Gilibrator is a battery-operated, electronic bubble flowmeter that provides instantaneous air flow readings and a cumulative averaging of multiple flow measurements. The unit consists of a flow cell assembly, control unit (base), and battery charger. The flow cell assembly consists of a flow tube. bubble generator, and sensor blocks located on each end of the tube. The Gilibratorwas calibrated by Gitian Instruments Corp. on February 2. 1993, using a film flowmeter (MCS-102) calibrator traceable to NIST, per circular No. 602. The flow rate of each sampling pump was calibrated before and after each use by attaching the flow celt (outlet) of the Gilibrator to the pump inlet with flexible rubber tubing. The appropriate sorbent tube (activated charcoal or silica gel tube) was placed in line between the GiJibrator and the pump. The bubble generatorwas activated on the flow cell to form a bubble film across the diameter the flow tube. The sampling pump draws the thin-film bubbles up the flow tube. As the bubble traverses past the two infrared sensors, each sensor transmits a signal to the control unit indicating the passage of the film. The control unit contains a crystal-controlled timing system, a microprocessor control system, and an LCD reading for displaying flow and other messages. The flow rate of the sampler is calculated by the internal microprocessor and displayed automatically on the LCD screen. Triplicate flow measurements were performed. The calibration results were recorded on the Air Sampling Data Sheet. During each experiment the following integrated air samples were collected: • One stationary sample inside the test chamber prior to each run for a period of 8 h (pretest background sample). • One air sample from the breathing zone of the test subject conducting the paint-stripping procedure (personal breathing zone sample). • Two stationary air samples within the test chamber for the duration of the paint-stripping task**(Iength~of-task** 

### sample).



### 21

### • One stationary air sample within the test chamber, beginning at

### the start of the paint-stripping task and running for an 8-h period (8-h, time-weighted average sample). • One stationary air sample outside of 

### the test chamber (supply air sample).



### 22 MRHJPPnA06-01

### SECTION 6 ANALYTleAl METHODS


### 6.1 MIDAC 

## FOURIER TRANSFORM INFRARED

## ANALYZER 6.1.1 Analysis ofthe Volatile Organic Solvents in the Paint StrIpper Airborne concentrations of the paint stripper solvents were measured in nearly real-time at the breathing zone 

### ofthe paint stripper applicator using a MIDAC Model 2400 Fourier transform infrared (FTIR) spectrometer. The instrument was equipped with a closed-path White cell with a path length of 20 m. Air from the breathing-zone of the product user was drawn to the White cell via Teflon tUbing with a GAST vacuum pump. Repetitive high-resolution spectra were collected and averaged at 4-min intervals over the range of 400 to 4,000 

## em" with resolution of 0.5 

## em". The FTIR spectrometer was operated from a portable computer. The FTIR was calibrated using a series of standards prepared in Tedlar gas sampling bags (Nutech Corporation). The standards were prepared by diluting an aliquot of appropriate solvent with high purity air to a volume of 20 L in Tedlar bags. The following chemical 

### were used for calibration of the FTIR:

• N-Methyl-2-pyrrolidonet 

### Aldrich Chemical Co" high purity, 99+%, HPLC grade • Toluene, Aldrich Chemtcal Co., high purity, 99.8%, HPLC grade • Acetone, Aldrich Chemical Co., high purity, 99+%, HPLC grade • Methanol, Aldrich Chemical Co., high purity, 99.9%
• Dichloromethane, Aldrich Chemical Co" high purity, 99.9%, HPLC grade • Dimethyl adipate, Aldrich Chemical Co., high purity, 99+% • Dimethyl glutarate, Aldrich Chemical Co., high purity, 98% The resulting concentrations of the standard series are presented in Table 5. The dilution volume was metered using a calibrated dry gas meter (Singer Company, MAl No. 9044) into clean, dry Tedlar gas sampling bags.



## 23

### Methylene chloride 

### 10, 100, 3,000 100 Acetone 

### 5,60,2,000 60 Toluene 

### 10, 100, 1,000 100 Methanol 

### 3,30,3,000 30 N-Methyl pyrrolidone 

### 30,60,180 60 Dimethyl adipate 

### 30,60,180 60 Dimethyl glutarate 

### 30,60,180 60 Dimethyl succinate 

### 30,60,80 60 Sulfur hexafluoride 

### 0.3,3.6 

### 3

Each Tedlar bag containing the standard series was attached to a sampling inlet and pumped into the FTIR White cell. Analysis of the samples was performed as detailed in Appendix B. A mid-point check standard (prepared independently from the standard series) was prepared and pumped into the White for analysis prior to each experimental run to monitor the accuracy and precision of the system over the entire project. If the analytical results of the check standard fell outside of the instrument performance objective, calibration of the FTIR was repeated with the full standard series.


### 6.1.2 Analysis of Sulfur Hexafluoride Tracer Gas Tracer gas concentrations within the test chamber were measured in nearty real-time using a MIDAC FTIR. Repetitive high-resolution spectra were collected and averaged every 

### 4 min over the range of 

### 400 to 

### 4000 em" with resolution of 

### 0.5 

## em", The FTIR was calibrated using a series of SF6 

### standards prepared in Tedlar gas sampling bags (Nutech Corporation). The TOOfar bags have Swagelok fittings that allow the injection of liquids or gases through silicone septa using Hamilton gastight syringes. A neat concentration of SF6 

### was prepared by 

### 24

### evacuating a 500-ml Tedlar bag and filling it with pure SFs 

### gas from a compressed gas cylinder (sulfur hexafluoride gas, Matheson Gas Products, > 

### 99.8% pure). Atiquots of the neat SFs 

### were drawn from the Tedlar bag using a Hamilton gastight syringe to prepare working standards. The series of SFs 

### standards in air were prepared by diluting aliquot of the working standard with high purity air to a volume of 20 L to produce standards in clean, dry Tedlar bags. The dilution volume was metered using a calibrated dry gas meter (Singer Company, MRI No. 9044). The resulting air concentrations of SFa 

### are presented in Table 5. A blank was prepared with the standard series using the preparation procedures specified above, except that no SFs 

### was injected into the Tedlar bag. Each Tedlar bag containing the SFs 

### gas standards and blank were attached to a Teflon sampling line and pump into the FTIR White cell. Analysis of the samples were performed as specified in Appendix B. A mid-paint check standard (prepared independently from the standard series) was prepared and pumped into the White cell for analysis prior to each experimental run to monitor the accuracy and precision of the system over the entire project. If the analytical results of the check standard fell outside of the instrument pertormance objective, calibration of the FTIR was repeated with the full standard series.


### 6.2 INTEGRATED AIR SAMPLES 

### Stationary integrated air sample and personal breathing-zone air samples were col/ected using the sampling methods presented in Table 4. Air samples were col/ected by drawing air through the appropriate solid absorbent tube (activated charcoal or silica gel) with a battery-operated, constant-flow pump. The sorbent tube samples were analyzed by DataChem Laboratories, Inc. using NIOSH methods, except for N-methyl pyrrolidone and the dibasic esters. N-Methyl pyrrolidone samples were analyzed using a method developed by GAF and partially validated by OSHA. The dibasic esters samples were analyzed using method developed by Du Pont. The analytical methods are presented in Appendix C. Immediately after sampling, the solid sorbent tubes were placed in a freezer at -18°C until they were shipped to DataChem Laboratories. The samples were shipped inside a foam-insulation container that was cooled with blue ice. Blind field spikes were shipped with the samples.



### 25

### where: 

### SEcnON 7 RESULTS AND DISCUSSION


### 7.1 INTEGRATED AIR SAMPLES The results of the integrated air sampling are presented in Tables 6 through 10 for each of the paint stripping products tested. The airborne concentrations are presented in units of milligrams per cubic meter of air (mg/m3) 

### and parts per million (ppm). The results in ppm were calculated using the following equation: ppm 

## = mg/m3 

### x 

### 24.5 M.W. M.W. = molecular weight of the analyte

24.5 

# = liters of vapor per mole of contaminant at 25°C and 760 mm Hg In Tables 6 through 8, the airsampling results for methanol are presented on a separate line from the corresponding results for the other organic compounds collected at the same location. Since methanol was collected on a separate silica-gel sorbent tube, the sample volumes are not the same as those for the other compounds. The first three paint stripping products that were tested contained two or more chemicals with relatively high vapor pressure (e.g., methylene chloride, acetone, methanol, toluene). The last two products tested contained one or more chemicals with lower vapor pressures (e.g., N-methyl pyrrolidone, dimethyl adipate, dimethyl 9Iutarate). Published occupational exposure limits for methylene chloride, toluene, methanol, acetone, and N-methyl pyrrolidone are presented in Table 11. No exposure limits were found for the dibasic esters. The threshold limit vatues (TLVs) are issued by the American Conference of Govemmental Industrial Hygienists (ACGIH). The permissible exposure limits (PEls) are regulatory limits promulgated by the Occupational Safety and Health Administration for working adults. The maximum concentration values (MAKs) are workplace standards set by Germany.

MRI-OPP1\R06-01 

## 27I\) (X) 

### Table 6. INTEGRATED AIR SAMPLING RESULTS-BIX STRIPPER

RunNo. 1 PrWstt.cIcQround 16 0480 148 71.0 NO (<0.1) NO (<0.06) NO (<0.1) NO (<0.04) Preliletbeckground 17 

### e> 149 71.5 NO (<0.1) NO « 0.1) T

.. ct..1bM, cenIiIr 19 48D 10.3 4.94 180 76 650 170 Test et.nber. ariIr 18 480 10.1 4.as 250 191 Testa.,_, iNMtide 23 128 24.8 3.10 310 130 870 230 Testc:MI ••,inIIIt

.... 22 126 25.8 3.25 920 703 Teetctwnbel, ouItItaide 21 126 25.9 3.26 310 130 

## aeo 230 Testdwnber, autIIItaide 20 126 31.1 3.92 760 581 BrwIhing zane 25 126 24.5 3.09 310 130 810 220 BAIlIfhingzone 24 128 29.7 3.74 750 574 SUpply

... 10testchamber 26 480 153 73.4 NO (<0.1) NO «0.06) NO (<0.1) NO (<0.04) 

### SuPDtY

...totMtctwnber 27 0480 148 71.0 NO '<0.1) NO 1<O.1l RunNG.2**Pree.t~** 29 48D 152 73.0 NO «0.1) NO (<0.06) NO (<0.1) NO (<0.04) PtWetbeckgrol.ni 28 480 151 n,S NO «0.1) NO «0.1) Test

# d*W_. cenw 35 480 10.6 5.09 180 80 630 170 Teactwnt.. centIr 34 480 9.2 •.4 290 220 TeachM_, inIIItaide 39 112 25.7 2.88 380 160 1000 270 Test ch8mber. inletside 36 112 26.2 2.93 1200 918 Testct..

__,outIM side 38 112 25.0 280 390 160 1000 270 Teetctwnber, outtlItside 37 112 25.8 2.89 1100 841 ere.4hlng lOne 33 112 24.6 2.76 310 130 830 220 8nMIthingzone 32 112 27.2 3.05 1100 841 Supply

..to
... chamber 30 480 156 74.9 NO (<0.1) NO (<0.05) NO (<0.1) NO (<0.03) 

### ISuclclIY lIirtotestcMnlber 31 480 152 73.0 NO (<0.1) NO (<0.1) RunNo. 3 P"'" bIcqround 40 480 151 72.5 NO «0.1) NO «0.06) 0.28 0.074 Pr8tIIstt.ckground 41 480 150 72.0 NO «0.1) NO«0.1) Testctwnb«. CWlW 47 480 10.8 5.18 230 100 600 160 Test etwnber, cenW 46 480 9.2 4.4 360 280 Teetct••

### *-, inIMtide 50 112 25.2 2.82 350 150 710 190 TestchImbeI. inlet

.. 51 112 25.7 2.88 800 612 T.-tet.nber, ouItItside 49 112 25.9 2.90 140 720 190 T_ctwnber. outletside 48 112 26.1 2.92 790 604 Brwthing zone 44 112 25.6 2.87 350 150 660 180 Br..chingzone 45 112 24.7 

### 2.n 790 604 Supply IIirtoWst ch8mbeI 43 480 153 73.4 0.3 0.1 1.4 0.37 

### SuPOlY airtotastchamber 42 480 151 12.5 NO (<0.1) NO (<0.1)N 

### co MRI-QPf'1\R06-01 

### Table 7. INTEGRATED AIR SAMPLING 

### RESULTS-SIX SPRAy-oN STRIPPER

Run No.4 bIIc:kQround**5~** 480 150 72.0 1 0.3**Pr*It~** 54 480 150 12.0 NO«O.1) NO«0.1) T
.. chwnber,canter 55JS6 480 10.8 5.18 1900 SSO Ttitchwnber,canter 57 480 9.7 4.7 160 120 T
..chM1ber, inlItside 61182 96 26.0 2.50 3100 890 

### r.. ctwnber, inlItside 63 96 26.2 2.52 2SO 190 T"dwnber, ouliIt Iide S&59 96 25.2 2.42 3100 890 TtitctIMIber, ouIIItside Sl 96 26.6 2.55 2SO 190 Bl-ehiIgZMe 67168 99 26.4 2.61 3000 670 8NIIlfqzone 69 99 204.9 2.47 200 150 Supplyiii'totestch8mber 64I6S 480 1<49 71.5 0.3 0.09 NO(<O.n NO(<0.1) 

### :SuDill¥IirtotestctlImber 66 480 151 12.5 RunNo.'**~~** 72/73 

# ... 153 13.4 1 0.3**Prt6IIIl~** 74 

# ... 151 72.5 NO«0.1) NO«0.1) 

### r.. dwnbIr.cerW 81/82 

# ., 9.9 4.8 1700 490 

# T. chM1I:ler, '*1W 83 

# ., 8.7 4.2 160 120 

# T. ctwnbw, inIIt

.. 15178 94 25.5 2.<tO 2900 6<tO T. ctwnbIr, ilIIttide 

### n 94 26.7 2.51 220 170 T. chImbIr, 0UIIt side 79180 94 26.0 2.44 3000 670 T. chMIber,outJlItslde 78 94 26.6 2.50 220 170 er.ttqzone 87181J 96 27.0 2.59 

# . .**~zone** 89 96 204.7 2.37 

# . . Supply.totielctwnber IW85 480 152 13.0 0.27 0.078 NO(<O.1l NO(<O.n**I~** 

### • to
.. chIImber 86 480 149 71.5 Run No.I PrWetbIdr;round 92193 

# ., 155 704.4 0.4 0.1**P"'~** 94 .-0 151 

### n.s NO«0.1) NO«0.1) TMtctwmer, center 9&'98 480 8.4 4.0 2000 580 T
.. chImber,center 97 480 1.2 3,5 170 130 T
..ctwmer, inIItside 101/102 92 26.2 2.41 3200 920 T
.. ctwnber. iIiItside t03 92 25.0 2.30 310 2-«) TettchMIDIr, editside 9Ml9 92 24.8 2,28 3600 1000 T. cfwnber.0IMetIIde 100 92 26.1 2.<tO 280 210 

### an.aqzone 10041105 92 26.8 2.47 3400 980 Breethfng

### zone 106 92 24.6 2.26 310 240 SuppI'fIirto testchamber 1071108 

# ... 161 n.3 NO«0.1) NO(<0.1) NO«o.n NO(<O.1) 

### suiJOlYIirto

.. c:hIrnber 109 480 158 15.8

• AirsamplerfailedcUIngrun.U> 

### o Table 8. INTEGRATED AIR SAMPLING RESUlTS-STRYPEEZE

RunNo.7 PreteltlJecIVound 113/114 480 151 

## n.S 1.5 0.43 NO«0.1) NO(<0.04) NO(<0.1) NO (<0.06) 

# P"'" bIlckgRIUnd 115 <480 151 

### n.s NO«0.1) NO« 0.1) Tfttctwnber, C*1ter 1221123 0480 8.4 4.0 230 70 240 64 130 55 Tatctwnber, eerier 12" 480 8.8 4.2 64 49 Testdwnber, in6It

.. 12Ot'121 107 25.2 2.70 370 110 340 90 260 110 TeetchImber. inIIt

.. 116 107 26.4 2.82 200 150 Tatc:hM1ber, outletside 1181119 107 25.2 2.70 300 90 230 61 180 76 TatchImber, outletside 117 107 25.8 2.78 210 181 8I'eIItqzone 12501126 6 26.2 0.16 

# . . . . . . Bl'elIIhlngzone 127 6 26.3 0.16 

# . . SUpplyairtotestchamber 128/129 480 152 73.0 1 0.3 NO«0.1) NO(<0.04) NO

### « 0.1) NO (<0.06) 

### SuPDIVairtotestchlImber 130 480 149 71.5 HOl<o.n Noe<O.l) Run No. I PnllwtbKtqJround 133/134 480 153 73.4 NO(<0.14) NO«0.04) NO (<0.1) NO(<0.04) NO(<0.1) NO (<0.06)**PnItIIIt~** 135 480 148 71.0 NO« 0.1) NO«0.1) TeMctwnber. eerier 13&'137 <480 9.1 4.4 270 80 300 80 160 61 T" dwnber. cerier 138 480 9.3 4.5 61 51 Teltc:twnMr,inIItute 142/143 110 25.3 2.78 470 1040 430 110 310 130 Tatc:hMlbIr,inIIIl

.... 144 110 26.5 2.92 2040 180 Tatc:Nmbw. ouattaide 14()j'141 110 25.4 2.79 490 140 430 110 310 130 

# T_chImber, outletside 138 110 26.0 2.88 240 180 8I'eIItqzone 1«il'1.es 110 25.6 2.82 430 120 390 100 280 120 8reIIlhing zone 147 110 25.1 2.78 230 180 Supplyairtolettchamber 1481149 480 145 69.6 0.1 0.03 NO

### « 0.1) NO (<0.04) NO«0.1) NO (<0.06) 

### IsuiXlIYIlrtotestch8mber 150 480 143 68.8 NO«0.1) NO«0.1) Run

# No.' PrMeatbKtqJround 153/154 480 147 70.6 NO (<0.14) NO(<0.04) NO (<0.1) NO (<0.04) NO(<0.1) NO (<0.06)**PretIIIIt~** 155 480 147 70.8 NO«0.1) NO«0.1) TeMchamber, center 15W160 480 9.1 4.4 230 70 250 66 130 55 TeltchImber. oenter 161 480 9.2 4." 68 52 T_cIwnber, inIIItside 185/166 118 25.2 2.97 400 120 340 90 2SO 110 Teltc:hMlb«. Inletside 189 118 26.4 3.12 83 63 TeltcNmbIr. outletside 16711f18 118 25.1 2.96 400 120 330 88 290 120 T" cMmber,outletside 170 118 25.7 3.03 190 150 BrwIIIt*Igzone 182/163 118 26.5 3.13 380 110 310 82 260 110 Brelthingzone 164 118 25.0 2,96 180 140 Supply

...totestchwnber 15&'157 480 U59 81.1 0.2 0.06 NO «0.1) NO (<0.03) NO«0.1) NO (<0.05) 

### IsuDdV

...to
.. chIImber 158 

# - 1f18 80.6 MOt<O.n MOt<O.n

•Airsemplerf1IIIedduringrun.

### cu



### ..... MAI-oPPM06-01 

### Table 9. INTEGRATED AIR SAMPLING RESULTS-WOOD FINISHER'S PRIDE

Run No. 10 PretestbtIekground 171 480 151 72.5 NO«0.1) NO«0.03) Testchamber, 

### center 172 480 148 71.0 

### 74 18 Testchamber, inlet side 174 126 148 18.6 38 9.4 Testchamber, outletside 173 126 150 18.9 45 11 Breathing zone 175 129 148 19.1 39 10 Suppty

### airto testchamber 176 480 150 72.0 NO«0.1) NO«0.03) Run No. 11 Pretestbedtground 192 480 148 71.0 1.7 0.42 Testchamber, center 193 480 26.1 12.5 46 11 Test chamber, inlet side 194 128 149 19.1 41 10 Testchamber, outfetside 195 128 147 18.8 42 10 Breathing zone 197 130 150 19.5 37 9.1 Supplvair to testchamber 196 480 145 69.6 NO«0.1) NO«0.03) RunNo. 12 PretestblIctcground 199 480 150 72.0 2.2**O.~** Teatchamber. center 200 480 25.9 12.4 46 11 Testchamber, inletside 202 139 

### 144 20.0 40 10 Testchamber. outletside 201 139 146 20.3 44 11 Breathing zone 204 143 145 20.7 37 9.1 Supplyair totest chamber 203 480 149 71.5 NO«0.1) NO«0.03)(,,) I\)

MRI-OPPl\R06-01 

### Table 10. INTEGRATED AIR SAMPLING RESULT5--3M SAFEST STRIPPER 

# IIlr:':Lr

Run No. 13 Pretest background 221 480 152 73.0 NO «0.01) NO«0.1) 0.16 0.02 Test chamber, center 222 480 26.1 12.5 8.8 1.2 4.2 0.64 Test chamber', inlet side 223 187 145 27.1 7.0 1.0 4.0 0.61 Test chamber, outlet side 224 187 149 27.9 6.8 1.0 3.9 0.60 Breathing zone 226 187 137 25.6 7.8 1.1 4.7 0.72 Supply air

### totest chamber 225 480 150 72.0 NO «0.01) NO «0.1) NO(<0.01) NO «0.1) Run No. 14 Pretest background 227 480 150 72.0 NO «0.01) NO «0.1) NO «0.01) NO «0.1) Test chamber, center 228 480 25.1 12.0 12 1.7 5.4 0.83 Test chamber, inlet side 231 176 145 25.5 9.0 1.3 4.7 0.72 Test chamber, outiet side 229 176 147 25.9 8.9 1.3 4.6 0.70 Breathing zone 232 184 121 22.3 9.4 1.3 4.9 0.75 SUDolv airtotest chamber 230 480 142 88.2 4.5 0.6 NO«0.01) NO {<0.1) Run No. 15 Pretest background 234 480 150 720 NO «0.01) NO«0.1) NO «0.01) NO «0.1) Test chamber, center 235 480 25.8 12.4 8.9 1.3 4.0 0.61 Test chamber, irnet side 238 184 153 28.2 8.5 1.2 4.6 0.70 Test chamber, outlet side 239 184 144 26.5 7.9 1.1 4.2 0.64 Breathing zone 237 186 145 27.0 7.8 1.1 4.1 0.63 Supply air to test chamber 236 480 143 68.6 NO «0.01) NO«0.1) NO «0.01) NO «0.1)

### Table 

### 11. OCCUPATIONAL EXPOSURE LIMITS

750 I 2380 I 1000 I 2400 I 1000 200 

### I C1885 

### I C500 

### I 375

400 I 100 100 100

200 360 380

260 2400 1 1000 150

250 560

325 100 250 200260 590 500 I C3480 IC1000

200 260 752 1740 150

250328 565 50 50

200 174 188

262 1780

ACGIH TLVs - American Conference of Govemmentallndustrial Hygienists Threshold Limit Values OSHA PELs - Occupational safetyand Health Administration**Permlssi~e** Exposure limits NIOSH RELs - National Institute for Occupational Safety and Health Recommended Exposure limits German MAKS - German Maximum Concentration Values in the Workplace TWA - Time-weighed average exposure concentration for a normal8-hour (TLV,PEL) or up to 10-hour(REL) workday. STEL - Short-term Exposure Limit is usually a 15-minutetime-weighted average exposure that should not be exceeded. Ceiling (C) - The concentration that should not be exceeded at any time.



### w c..> MRI-OPPl\R06-01

### The ACGIH TLVs are guidelines that are based on the best available information from industrial experience, and from experimental human and animal studies. These guidelines are intended for the workplace exposures for working adults and are applicable for the general population. The time-weighted average (TWA) exposure limit is the time-weighted average concentration for a nonnal 8-h workday and a 40-h work week, to which nearly all adult workers may 

### be repeatedly exposed, day after day, without adverse effects. The short-term exposure limit (STEL) is the air concentration to which workers can be exposed continuously for a short 

### period of time without suffering from irritation; chronic or irreversible tissue damage; or narcosis of sufficient degree to increase the likelihood of accidental injury or impair self-rescue. A SrEL is defined as a 15-min TWA exposure that should not 

### be exceeded at any time during a workday even if the 8-h TWA is within the TWA-TLV. The "pretest backgroundM 

### results represent the background air concentrations within the test chamber priorto each experimental run I 

### averaged over an 8-h period. The results demonstrate that the background air concentrations of acetone, methanol, and 

### the dibasic esters were below the detection limit 

### « 0.1 mglm3) 

### of the analytical method. The background concentration of N-methyl pyrrolidone (NMP) was belowthe detection limit prior to the first run in the series (run no. 10). The background levels measured prior to SUbsequent runs (nos. 11 and 12) were 1.7 and 2.2 mglm3
, 

### respectively. The N-methyl pyrrolidone background concentration appears to 

### be from low-level residual NMP in the test chamber from the previous run. The background air concentrations of methylene chloride and toluene ranged from below the limit of detection 

## « 0.1) to 1.5 mg/m3

. 

### Methylene chloride and tofuene were det$ded in the air supply to the chamber during some of 

### the runs; theretore, the background air concentrations measured prior to the runs may 

### be due eitherto the supplied air to the chamber or to residual chemicals from the previous run. In all cases, the pretest background air concentrations were low relative to the levets measured during the runs. The air concentration data were not corrected for the background. The first product tested in the ACE Laboratory was SIX Stripper, which contained acetone, toluene, and methanol. The air concentration of toluene measured in the breathing zone of the product user ranged from 660 to 830 

### mglm3

. 

### The stationary air samples collected during paint stripping and cleanup task (i.e., length-ot-task samples) ranged from 710 to 1000 mglm3

. 

### The 8-h TWA air concentration of toluene ranged from 600 to 650 mg/m3
, 

### which exceeds the PEL established by OSHA and the recommended limits pUblished by the ACGIH and NIOSH. 

### The ACGIH TLV for toluene is 188 mglm3 

### (8-h TWA). The OSHA PEL is 754 mglm3 

### (8-h TWA) with an acceptable ceiling concentration of 1885 rng/m3• 

### The breathing-zone concentration of methanol ranged from 750 to 1100 mglm3• 

### The length·of-task stationaJY samples yielded similar results ranging from 760 to 1200 mglm3• 

### Both the breathing-zone and length-of-task air concentrations for methanol exceeded the ACGIH short-term


### 34 MRI·OPPnR06-01

### exposure limit (STEL) of 328 mglm3
, 

### The 8-h TWA air concentration of methanol ranged from 250 to 360 mglm3
, 

### Two of the three 8-h time-weighted samples exceeded the ACGIH TLV-TWA for methanol of 262 mglm3
, 

### The acetone level were found to 

### be within occupational exposure limits. 

### The 

### breathing zone and length-ot-task air samples for acetone ranged 

### from 310 to 390 mglm3

. 

### The 8-h TWA sampling results ranged from 180 to 230 mglm3• 

### The SIX Spray-On stripper, which contained methylene chloride and methanol, was the only product 

### selected for

### this studythat was not applied with a brush. The stripper

### wassprayed onto the 

### ptywood substrate with a sprayer supplied with the product. The airbome concentrations 

### of methylene chloride and methanol measured in 

### the breathing zone of 

### the product user were found to be 3000 and 3400 mglm3•

### and 200 and 310 mglm3
, 

### respectively. The breathingzone sampler failed during run 

### no, 5 and was not reported. The stationary length-ot-task air samples ranged from 2900 to 3600 mglm3 

### for methylene chloride and from 220 to 310 mglm3 

### for methanol. The methylene chloride 8-h TWA air concentration ranged from 1700 to 2000 mg/m3
, 

### which exceeds the PEL set by OSHA (1740 mglm3) 

### and the recommended TLV published 

### by ACGIH (174 mglm3) . 

### The 8-h TWA air concentration of methanol ranged from 120 to 130 mglm3

. 

### Strypeeze, the third product tested, contained methylene chloride, toluene, acetone, and methanol. The results of 

### the breathing-zone and stationary lengthof-task samples for methylene chloride ranged from 380 and 490 mglm3

. 

### The breathing zone sampler failed dUring run no. 7 and was not reported. The 8-h TWA air concentrations ranged from 230 to 270 mglm3
, 

### which exceeds the ACGIH TLV-lWA for methylene chloride (174 rngIm3) . 

### The results of the breathing-zone and stationary length-of-task samples for toluene ranged from 

### 230 and 430 mglm3• 

### The 8-h TWA air concentrations ranged from 240 to 300 mglm3
, 

### which exceeds the ACGIH TLV-TWA for toluene (188 mglm3) . 

### The levels of airborne acetone and methanol were both within published occupational limits. The 8-h TWA air concentrations of methanol and acetone ranged from 64 to 68 mg/m3 

### and 130 to 160 mglm3
, 

### respectively. Wood Finisher's Pride, which contained N-methyl pyrrolidone (NMP), was the fourth product tested. The air concentration of NMP measured in the breathing zone of the product user ranged from 37 to 39 mglm3

. 

### The stationary air samples collected during paint stripping and cleanup (i.e.,length-of-task samples) ranged from 38 to 45 mg/m3• 

### The 8-h TWA air concentration of NMP ranged from 46 to 74 rng/m3
, 

### These results are higherthan those found during a study conducted in 1991 by the GAF Chemical Corporation of a similar NMP paint stripping product (Hylan, 1991). Airbome concentrations of NMP of 7.3 and 6.1 mglm3 

### were measured at distances of 1 and 2 

### ft, respectively, dUring the application of the paint stripperto a 40- by 30-in plywood sheet. In 1987, GAF researchers measured airborne concentrations of NMP during the removal at flocr-tlle adhesive from a 4- by 4-ft section of a concrete basement floor (Hylan,

MRI-QPPnR06·01 

## 35

### 1989). NMP air concentration in the breathing zone of the worker was found to be 2.3 mglm3• 

### The air exch8nge rates during these 

## tests were not specified. The air concentrations 

### of NMP were 

## wett betow

### the maximum concentration value in the 

### workplace (MAK) of 400 mglm3 

### 8lItabti8hed by Germany. Exposure limits for NMP have not been established by OSHA, NIOSH, orACGJH. 3M Safest Stripper, the final product tested, contained dibasic esters (dimethyl adipate and dimethyl glutarate). The air concentration at the breathing of the product user ranged 

### from 7.8 to 9.4 mglm3 

### for dimethyl adipat., and from 4.1 to 4.9 mglm3 

### for dimethyl glutarate. 

### The length-of·task statjonary samples ranged from 6.8 to 9.0mglm3 

### for dimethyt adipste, and from 3.9 to 4.7 mglm3 

### to dimethyl glutarate. 

### The a.h TWA air concentrations were slightty higher than the length-of-task results, ranging from 8.8 to 12 for dimethyt adipate, and from 4.0 to 5.4 for dimethyl gkJtarate. Exposure limits for the dibasic esters have not been estabJished by OSHA, NIOSH, or ACGIH.


### 7.2 HEARLY REAL-TIME AIR SAMPLES The air concentration of each of the target compounds were plotted against time. The plots for each experimental run are presented in Appendix D. The air concentrations of both the volatile and semivojatile compounds appeared to rise rapidly wjthin 

### the test chamber during the paint stripping operations. After the stripper operation was completed, the air concentration of the less volatUe compounds decreased at a lower rate relative to the more volatile components. The semivolatile compounds appeared to adsorb andlor absorb onto the test chamber surfaces. This Msink effect" extended the decay of the less volatile components overtime. The infrared spectra for dimethyl adipate and dimethyl glutarate were too similar to be resolved by the FTIR. The air concentration of total dibasic esters is plotted against time. The NMP air concentration data collected during run no. 11 sharply increases at approximately 2.7 h into the run. The vacuum in the White cell was above 2 in. Hg dUring the first period. The vacuum was corrected at 2.7 h by the FTIR operator. All data collected prior to the adjustment have a negative bias. The air concentrations measured by the FTIR appeared to agree with the integrated samples, with the exception of N-methyl pyrrolidone. The FTIR NMP air concentration data were higherthan the data measured by the integrated air sample results. This may have been due to difficulties in preparing standards of semivolatile compounds in air. The NMP that was injected into the Tedlar bag may not have fully vaporized due to saturation. This would have created positive bias to the data.



### 36 MRI-Of>PT\R06-01

### A combined plot of 

### the air concentration vs. time for experimental run nos. 3, 6, 9, 12, and 15 is presented in AppendiX 0, pg. 0-18. This plot presents comparative air concentrations levels of 

### thetarget compounds for all five paint stripping products tested. 

### 7.3 QUALITY CONTROL SAMPLES Blind spikes samples were prepared at MAl and submitted to DataChem Laboratories, Inc. with the regular air sampling media. The blind spikes were prepared by injecting a known votume of each of the target anatytes onto the appropriate sorbent tube with a microliter syringe. Table 12 presents the results of the spiked samptes as reported by DataChem. The percent accuracy, averaged over the three spike levels, were within an acceptable range (80% 

### to 120%) 

### for all analytes, except for dimethyl adipate. The percent accuracy for the dimethyl adipate ranged from 57% to 147%. In general, the accuracies of the more viscous semivolatile spikes were less than the accuracies of the volatite spike samples. The difficulty of delivering microliter quantities of a viscous chemical to the sorbent tube may have contributed to a wider accuracy range for the semivolatile compounds.


### 7.4 QUALITY ASSURANCEACTlVmES A system audit was conducted by the Senior Quality Assurance Officer during an experimental run in the ACE Laboratory. No systematic bias was found. An audit of randomly selected data was conducted and the project report was reviewed by the Senior Quality Assurance Officer.

MRI-oPf'MOtHl1 

### 37

### Table 12. BLIND SPIKED SAMPLE RESULTS

Methylene

### Chloride**1~** 

### 1.0 1.3 1.4 7.7 108**MoI.~.** 

### = 84.93 185 4.0 5.3 5.2 -1.9 98 

## Den = 1.325 186 7.0 9.3 9.0 -3.2 97 Acetone 

### 181 1.0 0.79 0.72 -8.9 91 MoI.INf.

# = 58.08 182 

### 6.0 4.7 4.7 0 

### 100 Den 

### = 0.791 183 10 

### 7.9 7.7 -2.5 98 

### Toluene 178 1.0 0.87 0.89 2.3 102 MoI.INf. :=: 

### 92.14 179 

### 2.0 1.7 1.7 0 100 Dena 

# = 0.867 180 4.0 3.5 3.3 -5.7 94 

### Methanol 189 1.0 0.79 0.76 -3.8 96 

### MoI.INf. 

### = 

### 32.04 190 2.0 1.6 1.6 0 100


### = 0.791 191 4.0 3.2 3.0 -6.3 94 

### N-MMhytPyrrolldone 241 1.0 1.0 

### 0.9 -10 90**MoI.~.** 

# = 99.13 242 1.5 1.5 1.7 13 113 Denali 

### = 1.033 243 2.0 2.1 2.4 14 114 Dlmethytatutarate 247 0.5 0.54 0.67 24 124 MoI.IM. 

### = 160.2 248 1.0 1.1 1.2 9 109


### = 1.087 249 1.5 1.6 1.9 19 119 DlmethytAdlpate 244 0.5 0.50 0.73 46 

### 146 MoI.WI. = 

### 174.2 245 1.0 1.0 

### 1.3 30 130


### = 1.0063 246 1.5 1.5 0.85 -43 

### 57



## 38 MRI-oPP1\R06-01

### SECTION 8 CONCLUSIONS


### Due to concerns about the toxicity of methylene chloride, chemical paint strippers with new fonnulations are currently available at some retail stores. Some of these new formulations reduced the methylene chloride content by adding other volatile organic chemicals to the mixture, such as acetone, methanol, and toluene (e.g., Strypeeze and SIX Spray-On Stripper). Other formulations contain mixtures of volatile organic compounds and no methylene chloride. SIX Stripper, which contains acetone, toluene, and methanol, is an example of this type of formulation. Other new formulations have been developed that contain less volatile compounds, such as N-methyl pyrrolidone (Wood Finisher's Pride) and dibasic esters (3M Safest Stripper). These new formulations were tested in a controlled environment to assess consumer exposures to these new formulations. The air exchange rate (ACH) selected for this study represents the ventilation rate of a closed room within a typical residence. Using chemical paint strippers in an environment that lacks adequate ventilation represents a "worst-case" situation and is not recommended by product manufacturers. The results of this study indicate that airborne exposures to paint stripping products with reduced methylene chloride content may exceed occupational exposure limits when the paint strippers are used in unventilated residential rooms. Airborne exposures to substitute compounds, such as toluene and methanol, were found to exceed occupational exposure limits when used with low ventilation rates. In addition, the new formulation substitutes a nonflammable chlorinated compound with flammable organic chemicals, such as toluene, acetone, and methanol. As expected, the formulations with the less volatile substitutes resulted in lower airborne exposures; however, the toxicity of these compound are less known. No U.S. occupational exposure limits have been set for N-methyl pyrrolidone, dimethyl adipate, or dimethyl glutarate; however, a maximum concentration limit for N-methyl pyrrolidone has been by established by Germany. The N-methyl pyrrolidone airborne concentrations generated during this study did not exceed this exposure limit.

MRI-OPI'1\R06-0t 

## 39

### The lower volatile compounds (N-methyl pyrrolidone and dibasic esters) appeared to adsorb and/or absorb onto the surfaces of the test chamber. At the completion of the paint stripping operation. the air concentrations of N-methyl pyrrolidone and dibasic esters decayed at a lower rate relative to the more volatile compounds. A higher number of air exchanges is required to reduce the air concentrations of lower volatile compounds to background levels after the paint stripping operation is completed. This ·sink effecf' may extend the duration of exposure of these compounds to bUilding occupants. Airbome exposure limits for N-methyl pyrrotidone and dibasic esters should be established for the general public (consumers) and in the workplace based on currently availabte human exposure and animal studies. The fire risk of the formulations containing acetone. toluene. and methanol also should be evaluated.

40

# secnoN9 REFERENCES Girman, 

### J. 

## R., and 

### A. T. Hodgson (1986). "Source Characterization and Personal Exposure to Methylene Chloride for Consumer Products." Proceedings 79thAnnualMeeting oftheAirPollution ControlAssoc. 

### Paper No. 86-52.7. Hodgson, A. T., and 

### J. A. Girman (1987). "Exposure to Methylene Chloride from Controlled Use of a Paint Remover in Residences." Proceedings 80th Annual Meeting ofthe AirPollution ControlAssoc. 

### Hylan, 

### A. C. (1991). Correspondence to F. Fusiak. 8 March 1991. Hylan, 

### R. C. (1987). Correspondence to P. Taylor. 26 March 1989. Matthew, T. G. (1987). "Environmental ChamberTest Methodology for Characterizing Organic Vapor for Solid Emission Sources." Atmas Environ 

### 21:321-329. McHugh, 

### J. M., and 

### K. M. Bauer (1992). "Indoor Air Quality Sink Chamber Tests.' Environmental Protection Agency, Office of Pollution Prevention and Toxics, Washington, DC. EPA 

### 600/R·92-094. "Guide to Occupational Exposure Values." Compiled by the American Conference of Governmental Industrial Hygienists. 1990. "Threshold Limit Values for Chemical Substances and Physical Agents and Biological Exposure Indices." American Conference of Governmental Industrial Hygienist. 1993-1994.

MRI·QPP1\R06-o1 

### 41

### APPENDIX A


### LIMITED SHELFSURVEY OF PAINTSTRIPPING PRODUCTS IN THE KANSAS CITY METROPOLITAN AREA

A-1

## Limited Shelf Survey of Paint Stripping Products in the Kansas City Metropolitan Area Product Name: Bix Tuff Job 

### Remover Product Number: 14002, #7485680220 Manufacturer's Name and Address: Bix Manufacturing Co, Inc. 

### P.O. Box 

### 69 Ashland City, Tn 37015 Contents 

### Listed on Label: 

### Methylene Chloride 

### Methanol Product Found at: 

### Ace Hardware 

### Payless Cashways True Valve Hardware 

### Product Name: Six Stripper 

### Product Number: 1002, 

### # 74856 10220 Manufacturer's Name and Address: Bix Manufacturing Co, Inc. 

### P.O. Box 

### 69 Ashland City, Tn 37015 Contents Listed on Label: 

### Methanol Toluene 

### Acetone 

### Product Found at: Ace Hardware 

### Paylass Cashways True Value Hardware

MRI·OPPTIR<J6..01 

### A-3

### Product Name: Bix Spray on Stripper 

### Product Number: #74856 60220 Manufllcturer's Name and Address: Bix Manufacturing Co, Inc. P.O. Box 69 Ashland City, Tn 

### 37015 Contents Listed on Label: Methytene Chloride Methanol 

### Product Found at: True Value Hardware Sherwin-Williams 

### Product Name: Goof off Product Number: # 

### 23494 00005 Manufacturer's Name and Address: Atlanta Sundries Lithonia Ga 

### 30058 Contents Listed on Label: Xylene 

### Product Found at: Payless Cashways Sears True Value Hardware Sentry Hardware 

### Product Name: Oops 

### Product Number: # 

### 33873 00045 Manufacturer's Name and Address: Diy Products Division Rhodes American 

### 2825 W. 31 st Street Chicago 

### II 60623 Contents Listed on Label: Ethanol Vm&P Naptha Xylene Monochlorotoluene 

### Product Found at: True Valve Hardware


### A-4 MRI.()PPT\R06-01

### Product Name: Klean-Clean 

### Product Number: # 30192 07399 

### Manufacturer's Name and Address: Klean-Strip Division of W.m. Barr Inc. Memphis, Tn 38101-1879 

### Contents Ll8ted on label: Xylene Methylene Chloride Ethylene Glycol Monobutyl Ether 

### Product Found at: True Value Hardware


### Product Name: Formby's 

### -Wood Formula- Paint Remover 

### Procluct Number: # 32053 30035 

### Manufacturer's Name and Address: Thompson and Formby Inc. P. O. Box 

### 667 Olive Branch, Ms 38654 

### Contents Listed on Label: Methylene Chloride Methanol 

### Product Found at: True Value Hardware


### Product Name: Powder/Plus+ Paint Stripper 

### Product Number: # 

### 2704600421 

### Manufacturer's Name and Addre.s: H.f. Staples and Company,inc. Merrimack, Nh 03054 

### Contents Listed on Label: Sodium Carbonate Calcium Hydroxide 

### Product Found at: True Value Hardware

### Product Name: Safest Stripper 

### Product Number: # 

### 5111 10101 Manu1llcturer'. Name and Add

.....: Do-It-Yourself Div 3m Consumers Product Group Box 33053 St. Paul, Mn 55133-3053 

### Contents Listed 

### on Label: Dimethyl Adipate Dimethyl Glutarate 

### Product Found 

### at: Payless Cashways Ace Hardware True Value Hardware Sherwin-Williams Servistar Hardware


### Product Name: Klean Strip Paint Remover 

### Product Number: Ks-221, # 5111 10101 

### Manufacturer'. Name and Addre.s: Klean-Strip P.O. Box 1879 Memphis, Tn 

### 38101 Contents Listed 

### on 

### Label: Methylene Chloride Isopropanol Ethanol Methanol 

### Product Found 

### at: Ace Hardware

### Product Name: Strypeeze 

### Product Number: # 49542 01102 

### Manufacturer's Name and Address: Savogran P.O. Box 130 Norwood, Ma 02062 

### Contents Listed on Label: Methylene Chloride Acetone Toluene Methanol Petroleum Distillates 

### Product Found at: True Value Hardware Ace Hardware Sherwin-Williams


### Product Name: Zip Strip 

### Product Number: # 38514 

### 72004 Manufacturer'. Name 

### and Address: Star Bronze Company P.O. Box 2206 Alliance, Oh 44601 0206 

### Contents Listed 

### on Label: Methylene Chloride Methanol Ethanol Mineral Spirits 

### Product Found 8t: Payless Cashways Ace Hardware True Value Hardware Beverly Lumber Sentry Hardware**"'Rl~'** 

### A-7 

# I

### Product Name: Wood Finisher's 

### "Pride" Paint Stripping Gel 

### Product Number: # 

### 54000 76520 Manufacturer's Name .net 

### Address: Creative Technologies Group Greenville, Sc 

### 29601 Contents Listed on Label: N-Methyl PyrrOlidone 

### Product Found at: Sears True Value Hardware Graggs Paint Co.


### Product Name: Nasca Liquid Stripper Paint and Wamish Remover 

### Product Number: # 

### 737n 07120 M8I1ufacturer's Name and Address: National Solvent Corp. Medina, Oh 

### 44256 Contents Listed on Label: Methanol Methylene Chloride Acetone Toluene Mineral Spirits 

### Product Found at: Sears


### Product Name: Quick Strip Refinisher 

### Product Number: 4002, # 

### 74856 30220 Manufacturer's Name and Address: Bix ManufactUring Co. Inc. P.O. Box 

### 69 Ashland City, Tn 

### 37015 Contents Listed on Label: Methanol Toluene Acetone 

### Product Found at: Payless Cashways 

## A-a MRI·QPPl\R06-01

### Product Name: Klean Kutter liquid Paint Remover 

### Product Number: Kk-5 

### # 3019200515 

### Manufacturer's Name and Address: Klean Strip Memphis, Tn 38101-1879 

### Contents Listed on Label: Methanol Toluene Acetone Methylene Chloride 

### Product Found at: Payless Cashways Sutherlands Servistar Hardware


### Product Name: Sears Paint and Vamish Remover 

### Product Number: My62533 

### Manufacturer's Name and Address: Sears, Roebuck and Co. Chicago, 

### 1\ 60684 

### Contents Listed on Label: Methylene Chloride 

### Product Found at: Sears



### A-9

### Product Name: Enrich Paint and Varnish Remover Product Number: # 42909 40083 Manufacturer's Name and Addre.s: General Paint and Chemical Co. Division of Cotter and Co. 

### 201 Jandus Road Cary, /I 

### 60013 Contents Listed on Label: Methylene Chloride Methanol Toluene Mineral Spirits Product Found at: True Value Hardware
Product Name: Kutzit Paint and Varnish Remover Product Number: # 49542 01112 

### Manufacturer's Name and Addr.ss: Savogram Co. Norwood, Ma 02062 Contents Listed on 

### Label: Methylene Chloride Methanol Toluene Acetone Product Found 

### at: True Value Hardware Sherwin-Williams Sentry Hardware



### A-10 

# I

### Product Name: Ace Extra Strength Stripper 

### Product Number: Ace 1182, 

### # 82901 11825 

### Manufacturer's Name and Address: Ace Hardware Corp. Oak Brook, II 60521 

### Contents Listed on Label: Methylene Chloride Isobutane Isopropyl Alcohol Stoddard Solvent 

### Product Found 

### at: Ace Hardware


### Product Name: Ace liquid Stripper 

### Product Number: Ace 1118, 

### # 82901 11189 

### Manufacturer's Name and Address: Ace Hardware Corp. Oak Brook," 60521 

### Contents 

### listed on label: Methylene Chloride Acetone Methanol Toluene 

### Product Found at: Ace Hardware


### Product Name: Ace Heavy Bodied Stripper 

### Product Number: Ace 12058, 

### # 82901 12058 

### Manufacturer's Name and Address: Ace Hardware Corp. Oak Brook, II 60521 

### Contents Listed on Label: Methylene Chloride Xylene Methanol Toluene 

### Product Found at: Ace Hardware A-11 

# I

### Product Name: Zip Strip2 Paint and Finish Remover 

### Product Number: # 

### 38514 70032 MlII1ufacturer's Name and Address: Star Bronze Co. P.O. Box 

### 2206 Alliance, Ohio 

### 44601 Contents Listed on Label: No Components Were Listed on Label 

### Product Found at: Sentry Hardware


### Product Name: Duffy's Paint and Varnish Remover 

### Product Number: # 

### 50431 35753 Manufacturer's Name and Address: Duffy's Refinishing Co. Cedar Rapids, la 

### 52402 Contents Listed on Label: Methanol Toluene Methylene Chloride 

### Product Found at: Sentry Hardware


### Product Name: Zing Paint and Vamish Remover 

### Product Number: None Identified on Label. 

### Manufacturer'. Name and Address: C and M Coatings Division 

### the Valspar Corp Kansas City, Mo 

### 64127 and Minneapolis Mn 

### 55415 Contents Listed on Label: Methylene Chloride Methanol Ethanol Aliphatic Hydrocarbons Wax and Wetting Agents 

### Product Found at: Servistar Hardware 

### A-12 MRI·OPPT\R06-01

### Product Name: Parks Pro Stripper 

### Product Number: # 

### 75955 15140 Manufacturer's Name and Address: Parks Corp. SomersetMa 

### Contents Listed on Label: Methylene Chloride Toluene Methanol Stoddard Solvent Propylene Glycol Monomethyl Ether Ammonia Dipropylene Glycol Monomethyl Ether 

### Product Found at: Servistar Hardware


### Product Name: All Pro Marine Paint Stripper 

### Product Number: # 

### 21204 Manufacturer'. Name and Addr•••: All Pro Corp. Tampa FI 

### 33619 Contents 

### Listed on Label: Methylene Chloride Isopropanol Ethylene Glycol Monobutyl Ether Methanol 

### Product Found at: Gragg Paint Co.

MRH)PPM06-01 

### A-13 

# II

### Product Name: All Pro Semi Paste Paint Remover 

### Product Number: # 

### 21404 Manufacturer's Name and Address: All Pro Corp. Tampa FI 

### 33619 Contents Listed on 

### label: Methylene Chloride Methanol Xylene Toluene 

### Product Found at: Gragg Paint Co.


### Product Name: All Pro Sprayable Paint Remover 

### Product Number: -# 

### 21924 Manufacturer's Name and Address: All Pro Corp. Tampa 

### FI 33619 Content. 

### Listed on Label: Methylene Chloride Isopropanol Ethanol Methanol 

### Product Found at: Gragg Paint Co.


### Product Name: All Pro Heavy Body Paint Remover 

### Product Number: -# 

### 21104 Manufacturer'. Name and Address: All Pro Corp. Tampa FI 

### 33619 Contents Listed on label: Methylene Chloride Isopropanol Ethanol Methanol 

### Product Found at: Gragg Paint 

### Co. A-14 

# I

### Product Name: Super Strip 

### Product Number: SSc, #49542 01132 

### Manufacturer'. Name 

### and Address: Savogran P.O. Box 

### 130 Norwood Ma 

### 02062 Contents Listed on Label: Toluene Methylene Chloride Methanol 

### Product Found at: Sherwin-Williams


### Product Name: SixQuick Strip 

# I

Product Number: 4002 # 74856 

### 30220 

### Manufacturer's Name and Address: Six ManUfacturing 

### Co. P. O. Box 

### 391 Old Hickory, Tn 

### Contents 

### Listed on Label: Methylene Chloride Methanol Toluene Acetone 

### Product Found at: Sutherlands

MRI-OPPT\R06-0\ 

### A-15Product Name: Klean-Strip Heavy Bodied Paint Remover Product Number:**Hb~2,** #30192 00210 Manufacturer's Name and Address: Klean-Strip Division W.m. Barr, Inc. Memphis, Tn 38101-1879 

### Contents Listed on Label: Methylene Chloride Ethanol Methanol Isopropanol Product Found 

### at: Sutherlands


### Product Name: Easy off Paint Stripper 

### Product Number: Sf-200, #3079220025 Manufacturer's Name and Address:**Klean~Strip** Division W.m. Barr, Inc. Memphis, Tn 38101-1879 Contents 

### Listed 

### on 

### Label: Alipahatic Dibasic Acid Esters Petroleum Distillates Product Found at: Sutherlands



### A-16 

# I

### Product Name: Strip-X Creamy Paint Stripper 

### Product Number: Sx-6, #3019200610 

### Manufacturer'. Name and Addres.: Klean-Strip Division W.m. Barr, Inc. Memphis, Tn 38101-1879 

### Contents Listed on 

### Label: Methylene Chloride Ethanol Methanol Xylene Product 

### Found 

### at: Suther/ands
Product 

### Name: Klean Strip Semi Paste Paint Remover 

### Product Number: Ks-3, #30192 00310 Manufacturer's Name and 

### Address: Klean-Strip Division W.rn. Barr, Inc. Memphis, Tn 38101-1879 Contents 

### Listed 

### on Label: Methylene Chloride Ethylene Glycol Monobutyl Ether Methanol Isopropanol Product Found 

### at: Sutherlands
Product Name: Plasti-Kote Paint Stripper Product Number: 289, #7191500289 Manufacturer's Name and 

### Address: Plasti-Kote Medina, Ohio 44256 and Upland, ca 91786 

### Contents Listed 

### on Label: Methylene Chloride Product Found at: Sutherlands 

### A-17 

# IProduct Name: Klean Strip Aerosol Spray Paint Remover Product Number: Sr-72, #30192 07210 Manufacturer's Name and Address: Klean-Strip Division W.m. Barr, Inc. Memphis, Tn 38101·1879 Contents 

### Listed on 

### Label: Methylene Chloride Methanol Monyl Phenoxy Polyethoxyethanol Product Found at: Sutherlands



### A-18 MRI-OPPTIRQ6.01 

# I

### APPENDIX B
OPERAnNG PROCEDURES FOR THE MIDAC rnR CLOSED CELL SYSTEM 

# II

B-1

### Nearty real-time sampting 

### and analysis of air at breathing zone of the test subject was conducted using the 

### MIDAC FTIR in the closed-eell operating mode. The system is mounted on an optical bench and consists of: • 20-m unheated fixed-alignment White cell with a folded path mirror
• Nemst glower and power supply 

### • MIDAC spectrometer • Transfer mirrors (two) The optical components listed above were bolted to the mounting holes on the optical bench.
SETUP OF THE FT1R CLOSED CELL SYSTEM The follOWing procedures were used to set up the MIDAC FTIR closed-cell system:

• Tum on the power supply to the Nemst glower.

• Depress the ignitor button to light the glower (approximately 30 s). • Verify that the ZnSe wedged lenses (light yellow color) are installed on the cell and the spectrometer. • Dim the room lights and Visually align the beam so that it is reflected off mirrors through the cell and roughly centered on the spectrometer lenses.

• Flush the cell with dry nitrogen gas.

• Remove the breather cap from the MIDAC spectrometer and fill the detector with liquid nitrogen; do not overfill.

• Replace the breather cap.

• Connect the power supply and computer to the spectrometer.

• Power up the computer and determine the storage space remaining of the hard drive. About five spectra can be recorded for each megabyte of space available on the hard drive.

• Start the Labcalc program.

• Select the F2 function key or the backslash key on the computerto bring up the menu.

MRI·OPPT\R06-01

### • Select ENVIRONMENT and then DIRECTORY from 

### the menu. (NOTE: All Labcalc menu 

### choices can 

### be 

### setected by

### either moving the cursorto the desired item and pressing the ENTER key, or by pressing the first letter of the menu selection.)

• Enterthe path name of the subdirectory to which the data will 

### be recorded (Example: C:\LC\DATA). Always end the path name with the 

### "V' symbol (Example: C:\LD\DATA\).

• Select the F2 function key to bring up the menu.

• Select ARITHMETIC and then DOPROGRAM from the menu.

• Select the AUTOCOL program. • If the printer is attached to the computer, an immediate printed record of each analysis can be obtained by selecting YES when prompted. If NO is selected at the prompt, the analysis files will be recorded only to disk and will be briefly displayed on the computer monitor.

• Enter a short summary phrase and a four-cheracter code for each data set. This code will be included in each filename generated for the data set.

• Enter the number of the desired scans. The scan number will usually be set at 64 (about 4 min).
ALIGNMENT PROCEDURES FOR THE FTIR CLOSED CELL SYSTEM The following procedures were used to achieve the final alignment of the closedcell system:

• Select the ALIGN mode from the main menu.

• Select a RESOLUTION of 8 wavenumbers from the secondary menu. • No other menu items should be altered with the possible exception of GAIN. Normal gain should 

### be set at 1. Higher multiples (e.g., 2, 4, 8, etc.) are possible but are not recommended.

• Select ALIGN from the menu. The current interferogram signal will be displayed on the screen with continuous updates. 

# I

8-4

### • Observe the zero point of the interferogram. The zero point should 

### be stable at approximately 800 units. An unstable zero point or a reading greater than about 1,000 or less 

### than about 600 indicates a problem. To correct the problem, first verify that the autoscaling function has not malfunctioned by exiting the ALIGN mode and then reentering the mode from the main menu.

• Observe the peak-to-peak reading of the interferogram. The reading should be less than 30,000 units. A reading of 32,767 indicates that the detector signal is saturated. In this case, the gain must 

### be reduced (see Section 3.0). Peak-to-peak readings below 15,000 units indicate that the gain is too low; however, do not readjust the gain until the alignment of the mirrors has been optimized to obtain the maximum possible reading.

• SlOWly move the mirror pivots horizontally and vertically to obtain the maximum signal strength.

• Adjust the poslnon of the spectrometer mounting table to obtain the maximum signal strength. First, move the spectrometer 'eft and right, then rotate in place, and finally, adjust the vertical angle with the mounting feet.

• Repeat the series of adjustments (first to the mirrors and then to the spectrometer) until no further improvements in the signal strength is observed.

• With maximum signal strength set, readjust the instrument gain if the peak-topeak readings are not within the range of 15,000 and 30,000 units.

• Press the ESC key to return to the main menu. Once the maximum signal had been obtained, the optical alignment was not changed. 

### SErrlNG INSTRUMENT GAIN The following procedures were used to adjust the internal instrument gain: • Do not attempt to reset the instrument gain unless the sample cell contains clean, dry nitrogen gas. Lower gain readings are normal when introducing sample gases or when recording a background spectrum with the source off or blocked. Before attempting to reset the gain, verify that the gain setting on the ALIGN mode menu is set to 1. Higher multiples of 2 or more may be used to increase sensitivity, but this also increases the noise.

• Open the instrument case by releasing the four latches and lifting the cover straight up and off. 

# I

MRI-OPFnR06-01 

### B-5

### • Locate the pre-amp board positioned near the center of the case. A small jumper block is mounted on the board in one of the eight jumper positions labeled A through H. Each jumper position changes the gain by a factor of 1.5. To increase 

### the gain, repositton the jumper block to a higher position (toward the letter H). Moving the jumperto a lower position (toward 

### the letter A) reduces the gain. Avoid dropping the jumper block into the instrument electronics. • When the peak-to-peak signal is between 16,000 and 30,000 units, the gain is optimized.

• Carefully replace the instrument cover.
DATA COLLECTION The MIDAC FTIR spectrometer is not equipped with a modulated source beam; therefore, a background spectrum was obtained for each data set. The background spectrum is subtracted from 

### aU otherspectra and corrects for cell temperature effects. Background spectra were recorded for each data set, unless valid background spectra have 

### been recorded preViously. The following procedure were used to record a background spectra: • Select BCKGRND SELECT from the menu. • Block the source beam. • Select COLLECT NEW BCKG and then press ENTER when ready. • The system will automaticatty record and save the interferogram to the hard drive in a fife named "XXXXb.spc" where 

### MXXXXM is the four-character base filename selected dUring the setup procedure The single beam spectrum will be recorded in a file named I·XXXXbc.spc.II 

### • Flush the cell with dry nitrogen gas. • Remove the beam block. • Select REF SELECT and then COLLECT NEW REF from the menu to record the reference spectrum which will be saved to the hard drive in a file named XXXXr.spc and XXXXrc.spc. • Purge sample gas through the cell. • Select SAMPLE START from the menu and enter the number of sequential data sets to be recorded as well as the time interval between sets. For 64 scans the minimum interval should be approximately 300 s. 

# I

8-6

### • Enter the file path name for the sUbdirectory where the calibration files are located (usually C:\LC\QUANT\). Calibration filenames have a ."cl" file extension. • Enter the filename for the analysis result file. • Select the compounds to be calculated from the menu (maximum of nine entries). As each compound is selected, a "+11 

### sign will appear under the selection. If a mistake is made, use the CLR selection from the menu to clear the entire list. The selection process must then be started from the beginning. • Press the number "9" key to end selections. • When the READY prompt appears on the monitor, start recording the spectra by pressing any key. • As each set is collected, the interferogram will be displayed on the monitor and saved to the hard drive. The concentration data for each compound will be calculated using the library spectra and predefined calibration files, displayed on the monitor in units of ppm-meters, and saved to the hard drive. The air concentration is determined by dividing this value by the path length (20 m). • After the data set is completed, a new base name can be selected to start another set. 

# II

MRI·QI>Pl\R06-01 

### B-7

### APPENDIX C


### ANALYTleAl METHODS

C-1 

# ,.fORMULA: Table H.W.: Table 1

OSHA/NIOSH/ACGIH: Table 1 PROPERTIES: Table 1 KETONES I METHOD: 1300 ISSUED: 2/15/84 REVISION #l: 5/l5/89 

# I

COMPOUNDS: (Synonyms: acetone Table 1) cyclohexanone diisobutyl ketone SAMPLING 2-hexanone methyl isobutyl ketone 2-pentanone MEASUREMENT SAMPLER: SOLID SOR8ENT TUBE lTECHNIQUE: GAS CHROMATOGRAPHY, FlO (coconut shell charcoal, 100 mg/50 mg)!!ANALYTE: compounds above fLOW RATE: O.Ol to 0.2 L/min
acetone VOL-MIN: 0.5 L -MAX: 3 L llhui 1 L 10 L lDESORPTION: 1 mL CS2' stand 30 min ! !INJECTION VOLUME: 5**~L** SHIPMENT: HI8K must be refrigerated [lJ SAMPLE STABILITY: unknown FIELD BLANKS: 101. of samples

ACCURACY
RANGE STUDIED. BIAS and OVERALL PRECISION (sr): see EVALUATION OF METHOD lCOLUMN: glass (3.5 m x 6 mm), packed with 101. SP-2100 0.11. Carbowax 1500 on Chromosorb WHP !TEMPERATURE-INJECTOR: 250°C -DETECTOR: 300 °C -COLUMN: 50°C to 170°C @ 10 0/min !CARRIER GAS: N Z or He. 30 mL/min lCAlIBRATION: standard solutions of analyte in C52 !RANGE: 0.06 to 10 mg per sample [2J !ESTIMATED LOD: 0.02 mg per sample !PRECISION (sr): see EVALUATION OF METHOD APPLICABILITY: This is intended as a general method for the ketones listed above. If only certain compounds are of interest, the instrumental conditions can be changed to maximize instrument response for these compounds. INTERfERENCES: None reported. Alternate columns, e.g., 101. SP-2100 or OB-1 fused silica capillary. can be used. OTHER METHODS: This**~ethod** combines and replaces Methods 51. S18, S19 and 520 [3J, 5178 and S35B [41. and 1300 (dated 2/15/84).

5/15/89 1300-1 NIOSH Manual of Analytical Methods 

### C·3KETONES I REAGENTS: 1. Carbon disulfide (CS 2 )GC grade.- 2. Analytes, reagent grade. 3. Nitrogen. prepurified. 4. Hydrogen, dry. 5. Air, filtered, dry. ·See SPECIAL PRECAUTIONS. METHOD: 1300 EQUIPMENT: 1. Sampler: glass tube, 7 cm long, 6-mm 00. 4-mm 10, flame-sealed ends with plastic caps, containing two sections of activated (600 GC) coconut shell charcoal (front 

## = 100 mg; back 

## =50 mg) separated by a 2-mm urethane foam plug. A si1ylated glass wool plug precedes the front section and a 3-mm urethane foam plug follows the back section. Pressure drop across the tube at 1 L/min airflow must be less than 3.4 kPa. Tubes are commercially available. 2. Personal sampling pump, 0.01 to 0.2 Llmin, with flexible connecting tubing. 3. Gas chromatograph equipped with FlO, integrator and column (page 1300-1). 4. Vials. 2-mL, glass. PTFE-lined crimp caps. 5. Syringe, 10-J.lL, readable to 0.1 lJL. 6. Pipet, TO, l-mL. 7. Volumetric flasks, IO-mL. 

# --I

SPECIAL PRECAUTIONS: Carbon disulfide is toxic and a serious fire and explosion hazard (flash point = -30 GC); work with it only in a hood.
SAHPLlNG:

1. Calibrate each personal sampling pump with a representative sampler in line. 2. Break the ends of the sampler immediately before sampling. Attach sampler to personal sampling pump with flexible tubing. 3. Sample at an accurately known flow rate between 0.01 and 0.2 L/min for a total sample size of 0.5 to 3 L for acetone or 1 to 10 L for the other ana1ytes. 4. Cap the samplers and pack securely for shipment. SAHPLE PREPARATION:

5. Place the front and back sorbent sections of the sampler tube in separate vials. Discard the glass wool and foam plugs. 6. Add 1.0 mL C52 to each vial. Attach crimp cap to each vial. 7. Allow to stand 30 min with occasional agitation. CALIBRATION AND QUALITY CONTROL:

8. Calibrate daily with at least five working standards over the range 0.02 to 10 mg analyte per sample. a. Add known amounts of analyte to C52 in 10-mL volumetric flasks and dilute to the mark. b. Analyze together with samples and blanks (steps 11 and 12). c. Prepare calibration graph (peak area vs. mg analyte). 9. Detennine desorption efficiency (DE) at least once for each lot of charcoal used for sampling in the calibration range (step 8). Prepare three tubes at each of five levels plus three media blanks. a. Re-ove and discard back sorbent section of a media blank sampler. b. Inject a known amount (2 to 20 J.lL) of analyte or of a standard solution of analyte in C52 directly onto front sorbent section with a microliter syringe. c. Cap the tube. Allow to stand overnight. d. Desorb (steps 5 through 7) and analyze together with working standards (steps 11 and 12). e. Prepare a graph of DE vs. mg analyte recovered. 10. Analyze three quality control blind spikes and three analyst spikes to ensure that the calibration graph and DE graph are in control. 5/15/89

### C-4 1300-2 NIOSH Manual of Analytical MethodsMETHOD: !300 KETONE5 I MEASUREMENT: 11. 5et gas chromatograph according to manufacturer's recommendations and to conditions given on page 1300-1. Inject sample aliquot manually using solvent flush technique or with autosampler. NOTE: If peak area is above the linear range of the working standards, dilute with C52' reanalyze and apply the appropriate dilution factor in calculations. 12. Measure peak area. CALCULAnONS: 13. Determine the mass, mg (corrected for DE) of analyte found in the sample front (Wf) and back (Wb) sorbent sections, and in the average media blank front (Bf) and back (Bb) sorbent sections. NOTE: If W b > Wf/10. report breakthrough and possible sample loss. 14. Calculate concentration, C, of analyte in the air volume sampled, V (L):

EVALUATION Of METHOD: The methods were validated under NI05H Contract COC-99-74-45 [5]. Desorption efficiency was checked by spiking known amounts of the compounds (either neat or in solutions with C52) on coconut shell charcoal. Samples were generated for acetone, cyclohexanone, 2-pentanone, and methyl isobutyl ketone by heating a quantity of the liquid to just below its boiling point in a 3-necked, 500-mL round bottom flask. The compound was carried through a fixed-temperature condenser to the concentrations. Samples were generated for diisobutyl ketone and 2-hexanone using a syringe pump which delivered the compounds to a heated glass-lined inlet which was swept with nitrogen, carrying the vapor to the mixing chamber. Results were as follows: Overall Measurement Method Range, mg/m 3 Breakthrough1 Range. mglsample Compound [2-5] (srI (L) (sr) DE2
Acetone 51.127 1200 to 4500 4.3 2.4 to 14.2 0.86 (0.082) (0.024) Cyclohexanone S19 98 to 392 65 3.8 to 18.0 0.82 (0.062) (0.025) Oiisobutyl ketone 5358 145 to 582 44 1.8 to 7.0 0.91 (0.070) (0.032) 2-Hexanone 5178 188 to 790 >45 1.5 to 8.1 0.81 (0.053) (0.018) MIBK 518 208 to 836 17 2.1 to 8.3 0.91 (0.064) (0.008) 2-Pentanone S20 395 to 1570 19 3.5 to 14.0 0.90 (0.063) (0.011) 15% breakthrough. 0.2 Llmin at high end of concentration range in dry ai r , 2Averaged over mass range shown.

5/15/89 1300-3 NIOSH Manual of Analytical MethodsKETONES I METHOD; 1300 

# I

Low-level desorption efficiency checks showed the DEs to be 70% and 761. for 0.024 and 0.096 mg/sample respectively for cyclohexanone and 67% for 0.052 mg/sample of M1BK (2]. REFERENCES; [1] uall Report, Sequence #552B-J (NIOSH, unpublished, Oct. 2, 1986). {2] Williams, Karen, Desorption Efficiency Determination for Cyclohexanone and Methyl Isobutyl Ketone, NIOSH/MRSB, Unpublished (1986). (3] NlOSH Manual of Analytical Methods, 2nd. ed., V. 2, 51, S18, 519 and 520, U.S. Department of Health, Education, and Welfare, Publ. (NlOSH) 77-157-8 (\977). [4] Ibid, V. 3, S178 and 5356, U.S. Department of Health, Education, and Welfare, Pub'. {NIOSH} 77-157-C (1917). [5] Documentation of the NlOSH Validation Tests, U.S. Department of Health, Education, and Welfare, Publ. (NlOSH) 17-185 (\977), available as Stock No. PB 274-248 from NTIS, Springfield, VA 22\6\. [6] NIOSH Manual of Analytical Methods, 2nd. ed., V. 1, P&eAH 127, U.S. Department of Health. Education, and Welfare, Publ . (NIOSH) 17-157-A (1977). METHOD REVISED BV; Edward J. Slick, NIOSH/DPSE; methods originally validated under NIOSH Contract COC-99-74-45.

Table 1. General Information COlllpound (Syoooyms) A.cetone 2-Propanone; CAS #67-64-1) Cyclohexanone (CAS #108-94-1) Diisabutyl ketone(2.6,-dimethyl4-heptanane; CAS #108-83-8) 2-Hexanone (methyl n-butyl ketone; HBK; CA.S #591-78-6) Methyl isobutyl ketone (H1BK; hexane; isopropyl acetone; 4-methyl2-pentanone; CAS #108-10-1) 2-Pentanone (methyl propyl ketone; CAS #107-87-9) Formula (M.W, ) CH3COCH3 (58.08)

«CH3)2CHCH2.)lO ( 142.2.4)
CH3{CHZ)3COCH3 (100.16) {(H3)2(HCH2COCH3 ( 100. 16)

CHlHz'H2COCH3 (86.13) Properti es* liquid: ap 56 0(; d 0,79\ g/ml; VP 35.5 kPa (266 mm Hg) liquid; BP 155 

### oc; d 0.947 g/mL; VP 0.3 kPa (2 mm Hg) 1iquid; BP 169 0(; d 0.847 g/mL; VP 0.23 kPa (1.7 mm Hg) liquid; BP 127 0(; d 0.812 g/ml; VP 0.4 kPa (3 mm Hg) liquid; BP 1\7 0(; d 0.800 g/mL; VP 2.0 kPa (15 mm Hg)
liquid; BP laO 0(: d 0.81Z g/ml. VP 3.6 kPa (27 mm Hg) Exposure Limits, OSHA NIOSH ACGIH 750; STn lOaD 250 750; STn 1000 25 (skin) 25 (skin) 25 (skin) Z5 25 25

5 1 5 50; STEL 75 50; STn 75 50; STEl 75
200; STH ZSO 150 200; STEL 250 2.37

4.01

5.82

4.09

4.09

3.52
*Density @25 0(; VP @ZO 0(. 5/15/89 1300-4 NIOSH Manual of Analytical MethodsFQRIIIJLA:**~;** CH40 

### M.W.: 32.04

OSHA: 200 ppm HIOSH: 200 ppw; 800 ppml15 min [1] ACGIH: 200 PPQ: STEl 250 ppm (1 ppm 

## =1.310mg/ml • 

### HlP) 

### METHANOL IIlETHOO: 2000 ISSl£D: 2/15184

PROPERTIES: liquid: BP 64.5 

## °c; d 0.192 glml • 20°C; VP 15.3 kPa (115 mm Hg; 15.1' v/v) • 20°C; explosive range 6 to 36\ v/v in air 

# I

SYJOtYM$; carbinol; methyl alcohol: wood alcohol; rAS 167-S6-1. SAMPLING SNIPLER: SOl10 SORBEHT TleE (silica gel, 100 mg/50 11I9) FLOW RATE: 0.02 to 0.2 Llmin VOL-"IN: 1 l i' 200 ppm -fW(: 

### 5 l SHIMHT: routi ne 

### SAMPLE STABILITY: 6 weeks BlANKS: 2 to 10 field blanks per set BULK SAMPLE: desirable, 1 to 10 ml

RANGE STUDIED: 140 to 540 mg/m ll 

# en (S-L**s~les)** BIAS: not significant [2] OVERAll PRECISION (sr): 0.063 [2]**lTEQlfI~:** GAS CHROMTOGRAPHY, FlO 1 ANALYTE: methanol !DESORPTION: 1 ml water; stand 4 hrs 1INJECTION VOlI.IE: 5 loll !**TEfft:RAT~E-INJECTION:** 200 °C**-DETECT~:** 250 - 300 °C -COllA!: 80 °C !CARRIER GAS: HZ or He, 30 mllmin 1 !COLUMN: glass, 2 m x 2 Inn 10, 60/80 mesh Tenax GC or equivalent !CALIBRATIOH: solutions of methanol in water !RANGE: 0.1 to 6 11I9 per**~le l~STlMATEO**  LOO: 0.01 mg per sample [51 lPRECISION (sr): 

### 0.032 [2] I APPLICABILITY: The working range is 25 to 900 mgllIl (19 to 690 ppn) for a 5-L air**~le.** The method is applicable to ceiling detemtinations. At high concentrations of methanol or at high relative hllllldity, a large silica gel tube is required (700 mg front section). INTERfERENCES: None identified.**~itive** identification by _ss spectl"CJftetry Illly be necessary in Sale cases. Alternative gas chranltographic C01UM5, e.g.• SP 1000, SP-2l00 or FFAP are also confirmation aids. High relative h""idity drastically decreases the capacity of the**~ler.** OTHER METHODS: This method carbines and replaces Methods SS9 (3) and P&CNt 241 [4].
2/15J84 2000-1 

### C-7REAGENTS: 1. w.ter. distilled. 2. Methanol.* 3. Nitrogen, purified. 4. Hydrogen. prepurified. 5." Air. filtered. *See special precautions. "T.elI): 2000 EQUIPfIIENT: 1. S-.:>ler: glass tube. 1 

### an long. 4

.. 10. containing two sections of 20/40 mesh silica gel sep4rated by a 2

.... portion of urethane foam (front 

## = 1001119. back

=- SO MI). NJTE: At high relative hunidlty or high _thanal**~trations.** use a larger tube: 15 at long, 8 Am 10. with three sections of silica gel (100 IIISI. lSOmg. 150 1119). 2. Personal 5aq)ling**~.** 0.02 to 0.2 Llmin. with fl

..ible connecting tubing. 3. Gas chrcllllltograph. FlO, integrator and collJlll'\ (page 2000-1) . 4. Vials. glass. 2-ml. PTFE-lined criMp caps. 5. Syringe.**10-~L.** readable to 0.1 pl. 6. Volu.etric flasks, lO-ml.

SPECIAL 

### PRECAUTIONS: Methanol i5 flllllMble and a dangerous fire and explosion risk. It is noderately toxk by ingestion and inhalation.

SMPLING:

1. Calibrate each perSOf'lil SMPling with a representative**~ler** in line. 2. Break the ends of the sanpl.r ilmlediately before s.tq)ling. Attach**~ler** to per-sonal sampling 

### pump with flexible tubing. 3.**S~le** at an accurately known flow rate beu.en 0.02 and 0.2 Llmin for a total**~le** size of 1 to 5 l. 4. Cap the samplers with plastic (not rubber) caps and pack securely for shipment. SNfILE PREPARATICIt:

5. Place the front and back sorbent sections of the**~ler** tube in separate vials. Discard the glass wool and fOM! plugs. 6. Add 1.0 ml distilled water to e.ch vial. Attach crilq) cap to each vial. 1. Allow to stand 4 hrs with occasional agitation. CALIBRATICIt AND QUf\lITY a»ITROl:

8. Calibrate daily with at least flve NOrking standirds over the range 0.01 to 6 1119 methanol per**~le.** a. Add known iIlIOUnts of methanol to distilled water in lQ....ft. volunetric flasks and dilute to the

## _Me. b. AM.lyze together with $Mples and blanks (steps 11 and 12). c. Prepare c.llibration grlph (pINk

..... vs .....thanol)

. 9. Dete11lline desorption efficiency (DE) at least once for each lot of silica gel used for S4WJ1Pling in the calibrat;on range (step 8), Prepare three tubes at each of five levels plus three Media blanks. a. RenNe and dlscard back $Orbent sectlon of a .'a blank allPler. b. Inject a known amount of methanol direetly onto front sol"bent section with a microliter sydnge.

21lS/84 

### C-8 2000-2ME1lQl: 

### 2000 

# II

c. Cip the tube. Allow to stand overnight. d. Desorb (steps 5 through 7) and analyze together wittl working standards (steps 11 and 12). e. Prepare a graph of DE vs. IIg

..thana1 recovered. 10. Analyze three quality control blind spikes and three analyst spilces to insure that the calibration graph and DE graph are in control. ME:ASlREMENT: 11. Set gas chl"CllMtograph according to manufacturer's**~tions** and to conditions given on page 2000-1. Inject Ulq)le aliquot manually using solvent flush technique or with**aut~ler.** NOTE: If peak area is above the linear range of the wor1cing standircls, dilute ",ith distilled water, reanalyze and apply the appropriate dilution factor in calculations. 12. Measure peak area. CALCUlATIONS: 13. Detemine the mass, 

### mg (corrected for DE) of methanol found in the uqlle front 

## (w,> and back ("'b) sorbent sections. and in the average media blank front (8f) and back**(~)** sorbent sections. NOTE: If > Wf/lO. report breakthrough and possible**~le** loss. 14. calculate concentration. C, of methanol in the air volume sampled. V (l):



# ------------------------------------- EVALUATION OF METlfJO Method SS9 (3)was issued on January 11. 1975, and validated over the range 140 to 540 ••' at 2S ·C and 758 nm Hg. using S-l**~les** [2]. Overall precision. sr' was 0.063 with average recovery for 18**~les** 94.2\, representing a non-significant bias. The atlllospheres were generated by calibrated syringe pIM'P. Desorption efficiency**~s** 0.92 at 1.31119 methanol and 0.84 at 0.65 Ilg methanol per sawple. Breakthrough (51. on back section) occurred at 52 min when saMpling an atmosphere containing 541 

### mg/m' in dry air at 0.2 l/min. Additional data were gathered using a larger (700 mg front section) silica gel tube under high tulidity condit1ons; thew _re published In P&CAM 241 [4]. A**~rlson** of the data is consistent with a recommended maximum sample volume of 5 L. 

### Front 8,...kthroullh Section, Test COnditions 

### capacity. Method f!IJ!I charcoal 

## 1..BH ms ..thanol 

### W. S59 [2.3] 100 5-40 0 5.6 10.4 P&CM 247 [4] 700 534 

## as 4.6 8.15

2/15184 2000-3 

# c-s!E!HQO: 2000 

# I

REFERENCES: [1] Criteria for a Recantnded Standard

...Occupational EXJlO$Ure to !'ethyl Alcohol, U.S.**Depl.r~t** of HHlth, Education, and Welfare, P\lbl. (..IOSH) 761-148 0(76). [2]**Doc~tation** of the NIOSH Validation Tests, U.S. Departllent of Health, Education, and Wt1fare, Publ. (NIOSH) 11-185 (1917). [3] NIOSH Ptanua1 of Analytlea1 P1ethods, V. 2, SS9, U.S. Depa.rtlnent of Health, Educat\on, and WtlfAre, Pub1. (NIOSH) 77-157-8 (\977). [4] Ibid, V. " NCNI 241, U.S. oepartment of Health, Education, and welfare, Publ. (NIOSH) 11-151-A 0(77). 

### [5] 

### User check, 

### UBTL, NIOSH 

### sequence 14121-K (Unpublished, November 3, 1983). IlIEl'HOO REVISED BY: Charles**~ister,** NIOSHlDPSE; SSg orlginally validated under NIOSH Contract CDC-GG-74-4S.

211SIM 

### C-10FOfIIIUt.A:**CH~12** P1.W.: M.94
OSHA: 500

....; C 1000

... P 2GOO

... 

### NIOSH:**l~t** 

### feasible; potenti., urc\nogen [1] ACGIH: 50 JlIlII; suspect 

### CU'Ci

..... (l

... 3.47 ..,... • ITP) S1'NONYMS:**dichl~thMe;** CAS 1'JS..09-2. 

### SIftlIW SMPlER: SOLID SORIEJfT 1laE (2 coconut shell cMrc:oal tubes, 100 

### mg and 50 1IIg) 

### FLOW**~TE:** 

### 0.01 to 

### 0.2**~in** 

### VOl.

....IN: 0.5 l • 500 PPM -MX: 2.5 l SHIMMT: separate front and blckup tubes SNPlE STABILITY: not det,rwined 8lN1CS: 101 of s..,1es
ACCLUCY RMGE STUDIED: 1100 to 7097 MgIm. (l-l SaMples) [2] BIAS: 

### not significant 

### [2) OVERAll PRECISION 

### (sr): 0.073 [2] 

### """," 

# .... ...,.:

# ,. I$SIB: 211S114 REVISI. ,,: 

## "1SlI7
PROPERTIES: 1'quid; d 1.323 

### tIa • 20 

## -c; 8P 40 ·C;

.. -95 ·C; yP ., kPa (341 • 

### til; _ v/v) • 20 

## ec; not 

## n.....,.

!TECIIIlquE: GAS ctIINTOGRAPHY. FlO ! I1Mlm:

..thyl.ne chloride ! !DESOIPTICII: 1 III CSZ. 

### sund 30 

### .tn ! !INJECTION VOUJIE: S lit ! !TBftMTURE-IIIIJ£CTlON: 200 to 225

## -e -DETECTOR: 2SO ·C -COUIII: 60 to 90 ·C !

### C1MIER GAS: HZ or He. 

### 30lILIJIin ! !COUIIt: 

### 3 • 

### x 3 _ 

### suinless st
..,. 101 

### SP-looo on 80/100 -.sh Ch,...sorb

... !eAlI_nON: standlrd soluttons of CHzC12 ! in CS2 "tth internll stAndard**!~:** 0.3 to 10 " per slMP,. [3] ! !E5TnMm LOO: 0.01 III pel" SIIllPle (••5] !PRECISION (sr): 0.026 , 1.3 to 5.3

.. 

## '-1" ! s-.ple (21 

# I

APPliCABILITY: The lIIDt"It:i

.. ,... h ,. to 3000 ,.. (350 to 10,400**~)** for a l..l air 

# se1,. l1!t .-tt!od 

### is .".,. " gUi. 

### dItnlMtions. INTalFEIlINCES: None identif'ed. 1'hI

...... WI 

### vaU.ted using I 

### 6 • x 3 _ statnless 

### st
.., col_ packed w;th lOS FFN' on 1001120 ..,,, SUpelcoport. AlternAte ChrGllltGgrlPhic col.-s are lOS TCEP 

### on 801100 Chramsorb Pllt. 5P-21oo. SP-21GO with O. carbcNu 1500. or 01-1 'usld 

### silica ctp;11arx 

### eolll!' OTHER ..eTl«JOS: This I"ftises "'thads S329 [3)

..'005 (dated 21lSIM), PSCM 121 [.]. and the criteria 

### doc:.-nt

..tttod (6]. OSM

...thod 59 uses larger {350",)sOrbent sections and has been .¥lluated for 10-Lair ,..les at 1 _ .",11M chloride [7],

8/1S/81 1005..1 MIOSH fllanual of Analyt\cal Pltthods 

### C-11

### MET!!'tJ.B CHLORIDE

1. E1

..

### t:

# -=-- disa1f1d1*.**~~tc** ..

### lily. COftutnh'lt 0.11 ,Iv decant. bInzaM or other sufUbl. internal studard. 2

....**~1** .. chloride. 3. IIttl"Clgln 

### or heli

.. purified. 4. H)1dNlln. p....rif

.... S. Air. filtered. CClIIPressed.


### -see SPECIAL PRECAUTIONS. 

### fITIII; ,. EQUlflftEIfT: 1.**~ler:** Hfalr.te frant Iftd bide

.. glus 

### tuMs with pllstic**~.** 7 

### c:. '011. ,_ aD. 4 _ 10. fl

__



## ...,ed

.... CGl\tlfnh'l Kth.tecI (MO ec) cocanat shill cMl"COIl (f,..t. 100

..; Melt • 50

..). A sHy11Ud glass ..-1 pl" is placed 

### at eIdl aM of 

### ..ee- tube. PNssuN drop across the tuMI 

### at 1 L/IItn .irl1c:w

..st be less thUI 3.4 Ie,•• Note: 1-.0 tIC IIrcillly..:.vanlbl. tubes, HCh canuining 150 III CMl'COil in 

## we. beds• .- be uMd. 2. PersoMl NIIlPltng pIlIP. 0.01 

### to 0.2 

### v.tn. 

### wtttl flexib1. COftRICting tubing. 3. Gis 

### cmo-totriPh. fl_ tOfttuttOft 

### .teetor.**in~tor** Iftd col_ (PIlI 1005-1). 4. 

## vi.ls. 2

.... mE-lined up_ 

### crt. CliPS. S. 

## syri.... lo-loll. rodIbl. to 0.1 loll. 6. Volu.etr;c fl.sks,**l~.** 

# II

SPECIAL PRECAUTIONS: carbon disulfide is tcucic and • s.rious fire Ind exp1ostoa buard (flash point., -30 ee); work with it only in • hood.
SMPll.:

1. calibrate udl persoMl HIlIIPHng

.... with

......sentltiv. HllP1ar in H
.... 2. 8rNt ends of UlllPler ;"i.t.,y before HllPli.... Connect the two SGr'Hnt tubes with a short piece of flexible tUbing. AtUch**~l.r** 

### to personal 5

..ling witll fl.tb'.**~tlg.** 3. s..le It In accurately kncMI flow rllte betwHn 0.01 Ind 0.2 LlJrin for a total $Mpl. size of O.S to 2.5 L. 4. separate tile front .nd kckup Wbes and e.tP

# Me" tube to ,revet .;gral;on of _thyl.- chloride betwen 

### tubes. ',ck securely for sMllltRt. SMI'lE PREPARATION:

S. PlIICe the front and back 

### sorbent sections (i

### .e., front .nd backup 

### tubes) of the 1MP'''' 

### in SfIPAr.te vials. Discard the glloss wool and fMl plugs. 6. Add 1.0

..... eluent to each vial. Atueh cri. cap 

### to Mch vill. 1. Allow to stand 30 .in with occaslOMl Agihtion. CAlIIMntll All) QlMUTY CClfTIQ.:

8. calibrate daily wfth at 'ent fhe working stMdlrds over tN r.,.. 0.01 to 10 III ._,.- chlorhle per UllPle.

. a. Mel kftOlllt .cMIItts of 

### _ttlyl.ne chlorhle to eluent in 104L YOl

...tric flasks'" dUm to 

## t_..n. b. Analyze toetther with slllPles and blanks (steps 11 _ 12). 

### c. ""re 

### calibration grAPh (ratio of peak Ioreaof 

### analyte to pHIl 

### area of 

### ;nte....., stMdM'd vs • .-g _thyl

.... chloride). 9. DeteNine desorption efficiency (DE) It lN5t once for Hch lot of cMrcoal used for ,.11ng in the calibration range (step 8). Prepare tine tubes at each of five leM1I plus 

### three Media blanks.

1115117

### C-12 1005-2 ..IOSH Kiftu41 of AM1yt\cal**~s**

## !I!W: 1005 

# I

A. 

## --.w...... disard bIck

.........t sectlOll of A
....i.. bl.**~l.r.** b. Illject A It..- 

### _t of .thyl

.... chloride diNCtly onto front sortIent section with a 

### lit

### croHter'

# sm"". c. CIp tM tIM. An

... 

### stall ov.....i

...

### t. 4. Desorb (steps 

### tInuIiI' 1)

.. 

### "'yn "ith worldng 

### stMdlrds (steps 11 and 12). 

### e........... A

# gr. of DE ft. III .thyl

.. chloride recowerwd. 10.**AMl~** thrM

..lily c.trol bHnd spikes

_ three a"""yst spikes to insure that the al;brAtion

# gr" Ind DE

# gr_ Ire in control. flJEASUFLiEJEiUT: 

### 11. 

## set lIS chr-.togr. according to
.....factur-.r·s Nee IndlU.S and to conditions given on ... 1005-1. Inject UlllPl. oiliquat IllnUlilly using solvent flush technique or vi th IUtosIIIpl.r. IIJT£: If peU 1m 

### ts
.. the 11

....1' ringl of the working stMdlrds. dilute vith .'uent, runalyz. and apply the wroPriAtI dilution fACtor in aleulltions. 12. flluu

... 

### PHk ArH. Divide the peak a

.... of analyt. by the peU a..... of intemal standlrel on 

### tew

# s_ ch

.....

### togr_. CALCUlATICItS: 13. DI\etWine the MSS. III (corrected for DE) of .thylene chloride found in the UIIIP" front (w,) and back (....) SOI"MIIt sections. Ind in the aver••lella blank front (8f) and Met (lit») sorbtnt sections. 'In'E: If

## Nt. > "'/10.

# ,...,.t brHkthrough

.... possible UlllPle loss. 14. Cllculate concentration. C. of _thylene Chloride in the air vol

.. s.-pl.ct. 

### v (L):

EVAL.lMTICil OF fETIIJD:

...thad S329 (3] .5 bsued on June 6. 1975. And VAlidated ower the ruge 1100 to 11GO ..".. It 25 

## -cand 163 _ Hg usi

.. I l-L $.-pl. [2). QIIerI11 prKtsion. sr'

# .s 0.013 .nth 

### lver. NCOMry 1S.1S

......tilll a non-signtfiant bill. The concentrltion of .thyl

... chloride

...s i

.....ntly verified by ClHbr.t.ct syringe,.... Desorption effic1Hey .s 0.91 in the 

# 1''''' 1.3 III to 5.3 III _tllyl

.. chloride per UIIP". Breakthrougll (SI on bKtt section) oce""'" at 18.5 .in lIIhIn Y1IPling an aamsphere containing 6126 IIg/III _thyl

.... chloride 

### at O.187 lilli

### n at OS RH. REFElHCES: [1] IJOSH 

## cu......t Ilttl1i.-ee

...11.tln.. filthy)

.. Qloride. 

## u.s. o.p.r-.nt of HHlth and

-.. Services. Publ. (IJOSH)

....

# 11. (,...n

# 1.. ,.). [2] Doc_ntation of 

### t. NJOSH validation 

### Tests. NJOSH. 

## sm. u.s. DIpa
......t of Hulth. 

### EMation. and

...

# ,f

.... Ml. (IIOSH) 11-185 (1911). [3) IJOSH "'nul of AnalytiCil "'tMds. 2nd ed., Y. 3. 5329, U.S. DIpI

.....t of HHltb. EduCltion, and

...,fa

..., ,.,. (IIOSH) 17-151-e (1917). [4] 110SH Rlnul of .'ytical 

### ;"tMds, 2nd

.... Y. 1. NCNI 121. U.S. DtpI

......

### t of Hulth. EdKltion

........,f

..... ,.,. (NJOSH) 71-151-.\ (1911). [5] User check. 

## _n, NI05M 

### n99O-R (

....,lshed. No""r 3. 1983). [6] Criteria for a Reca.l_d SUnArd.••occupational Exposure to
...thylene Chloride. 

## u.s, OtpIrtilftt of Health. Educat'on. and welfa

.... Publ. (NIOSH) 76-138 (1916).

1115111 1110511 KlnUl of ""'1)'\\cal Mhods 

### C-13

## !II1A;

# 1. , I

[1] 

### OSM Analytical ftlthods

....., 

### 0915'. avan.l. f". 

### ACGIH. 6500 GleNMy Ave•• Cincinnati. Off 45211. IlETHOO REVISED BY; G. DavidFall)'; .,. T. GIgnoft; and I. J. Wi11iMS. tlIOSHIDPS£; 5329 

### originally validated under 

### NIOSH COntract CDC-99-74-4S.

8/15187 

### C-14 lOO5-C NIOSH Pll.JlAl of AMlytical

...thods

# tl

F

....LA:

# a; C1Ks ".W.: 

### 92.14 IETHOD:

... 

### ISSUED: "15181
OSHA: 200,..; C 300 PIlII; P SOO

.... 

### NIOSH: 100

## ppn; 200 ""10 lrin [1.2] ACQIH: 100 PIlI; 150 PIlI 

### (STeL) (1 PIlI .. 3.17 MgIII8 • NTP) 

### PROP1:RTIES: 1iquid; d 0.866 g/IIL • 20 ·C; IP 110.6 ·C;

.. -95 ·C; yP 3.8 kPa (28 _ Mg; 3." v/v) , 2S 

### ·c; Ixplosive range 1.3 

### to 7.11 

### vlv in air 5Y111m1S: _thylbenzene. CAS '108-88-3. 

### MUNG SAMPLER: PASSIVE (Ictivated carbon) !TECHNIQUE: GAS CHRQIIMTOGRAPHY. FID


### SAMPLE TINE-'fIN: 15 .in • 200 -MX: 8 hr • 20 to 200 !ANAlYTE: toluene !DESORPTION: 1.5 Ill. clrbon disu1f1de; stand 30 .in SHJPPIEIfT: see step 2 - if necessary. trlnsfer sorbent pad to sept-..capped vial; otherwise. routine SAMPLE STABILITY: It lHst 2 .-.Ies • 2S ·C if stored in sept-...c:appect vial !INJECTUII VOLlIE: 5 pl !TENPERATURE-INJECTI01: 175 ·C -DETECTOR: 200 ·C

-tOUR: 100 ·C 

### FIELD 8l.N1(S: 101 of sMP1.s BULK 

### SNl'LE: desirable ACCURACY !CARRIER GAS: He or**~.** 30 JIIlIJDin ! !COUIII: 3.6 • x 3 _ 00 5P-looo on 80/100 mesh Chramosorb .-tP AMGE STUDIED: 15 to 2250

### 1IIlVWI- [3] 

### BIAS: not significant [3] !CALJRRATION: alNllyte solutions in CS2 ! !RMGE: 0.05 to 15 II!I per**~1e** OVERALL PRECISION (sr): 0.038 [3] !ESTIMTED lOO: 0.01 IIIg per**$~le** 

### !PRECISION (sr): 0.022 (3] !**-----------------~------------------** APPLICABILITY: The WOI"king r..... is 13 to MO (SO to 2500 ..,.-) for a**~hour** s.,le. The _thad is IPPHQbl. to ceili

.. _ten.hations. TM_thad deteraines toluene Vlpor only (not aerosol). tallpetitive adsorption by IMter vapor and other volatile organic solvents affects sMP'er apacity. INTERFEltENCES: None identt,ted. ThI chrc.,tographic co1_ or separation conentions rM'J be cMnged to circ

..ent interference probl_. OTHU fIETHOOS: 

### NIOSH

...thads 1500 and 1501 tlllployIcthe 5.,1;09 on charcoal tubes with overall sensitivity 

### about the Sale IS this

..thad.
8/15187 4000-1 

### NIOSH Kanua1 of 

### Ana1yt'cal**~thods** 

### C-15

### TQU8E REMENTS: 1. El..-t: oarbon disulfide**(C~).** 

## ee.r-t••ic qulity.* 2. 

### Tol_. rMgIIIt 

## gra. 3. Nitrogen or belhll. purified. 4. Hydrogen. prepurlfitd. 

### 5. Air. filtered. *See SPECIAL PRfCMITICIIS. 

### fIT!IW: .. EQUIPlI8T: 1. s.,ler: plssive 

### _itor "ith**~cU.atlld** cMrcoI1 

### collection .,....t. lIIDI'Iitors .st be 

### of k

.... SilIIP

### 1\.. rate for toluene. 2. Gas e 

### totr
.... flO. integrator and col

... ( 1). 3. Vi.ls. 

### ,lass. 2

...... 

### "it

.. PTFE-lil" sept

.. c.ps. 4. Pipet. TO, 1.S-4II.. and.pipet bUlb. 5. Syrifll". 5-. 10-. 2S- and lOO-lit. 6. Volu.etric flasks.**l~.** 

### 7. Tw.ezers. 

# I

SPECIAL PRECAUTIONS: brbon disUlfide is tode and extreltl)' fl

....,e (flash point. -30 -C); work with It onl)' in a hood.
SMPLING:

1. -..owe s_'er fl"lll pilCkage and rwm¥e CIPS if WlicAble. Atuclt UlllllPler in 

### wort
...·s brHthing zone. .... 

# s ..... u.pler 

# ",'.ts 'N UllGbstructed. Record start of s..Ung ti.. Follow-.nuflCturer·s ret'

.. nAtions to 811-.te appropriate SMPling 

### ti_ based on relative tuIIidlty**~nd** suspected coneentration of toluene. NOTE: The uptake constant is only valid for**~lers** in air with .'ent veloctty higlter than ca. 10 calsec. For.,...

# S,,'H. 1!MUf'e adequate air -.v_nt. l. Te
...inate sallpling by sealing the s.'. as Nee 8.nded by the -.nuf.c:turer or by transferrh'9. in a tol

...f

.... envit'OlKlftt. the IoCth.ttd charcoal collection .1_t to a vial and sealing the vial with a sept. Cip. Use weezers for hlndling the collecUon .'

..nt. taking care not to touch any activated cMrcoal. NOTE: 

## sm. s",'.r desi",s (e.g.• 3ft 35GI [4]) do not require transfer of the COllect1Oft el-.nt; otbers (e.g_. DuPont G-M and 6-18) require transfer of sorbent pad to I 5811ed vi.'. 5aIe s,,'er designs (e.g.• Druger ORSA-S) use granular sOfil,ent. SNl'LE PREPARATION:

3. Add 1.5 III CS2 to each collection el

...t. 

### 4. Allow to stand at least 30 .'n with 

### occlsional agitation. CAUBRATION AND QUALITY CONTROL:

5. calibrate daily whit at least five worti

... stMdards. a. Add known MIMIIIts of toluene to in 10.... vol

..tric fliSh and dilute to the 

### _rat to produce toluene concentrations itt tile range 0.01 to 10 1Ig/Itl. b. Analyze with s

...les and bla.s 

### (sqps • thl"OUlh 10). c. Prepare alibl-.tion

# tr.(

........ vs... tol

....). 6. Dete
...i. desorption efficiency (DE) in tM oalibr.tion range at least once for efd lot of $",'en used. Prwpare three

# ''''.rs at etch of fiye concentrations plus three -.lia blanks. a. Pl.ce the collection el_nt of a ••lia bl_ SIlIPler into

.. vial and ape b. Inject a kncMt

..nt of toluene directly onto the collection el

....t vith a .Icroliter syringe. c. Allow to stand overnight. d. Desorb (steps 3 .nd 4) .nd .nalyH with working standolrds. e. Prepare a graph of DE vs. ntg toluene recovered.

8/15/87 

### C-16 «)O()-2 NIOSH Manual of Analytical Methods

# I

1. Anllyze three**~l** ity control b1ind spik.s and th,. .ul)'St spikes to ensure that the 

### calibrltton gr. and DE
..... aN in control.**~:** 

### 8. 

## set gas cbf"altogr. accordi

.. to .nufKturer's 

### NCG.Lndltions and to conditions 

### ghen 011

..... 4000-1. 

### 9. Inject sa-ple 

### aliquot Mnua11y using 

### solvent fl.sh**~ique** 

### or with an 

### autOSllP'.r. tGTE: If puk area is abo" the Hnur range of 

### the ..wIting 

### standards, dilute an aliquot of the desorbed liquid w'th CS2' reanalyze, And apply 

### the appropriate dilution factor 

# 'n calculations. 10. 

### ....sure peak 

### arei.. CALCULATIONS: 11.**De~iM** the .ss, .. (corrected for DE). of toluene found on the s..

### le collection

.,....t 

### 00 and on the aver. 

### "'ia b1. (8). NOTE: If \II > s.IIIIP'.r "PICity • 0.33, 

### the SIIIlPler

_ be 

### saturated [6). 

### Evalui.te each 

### rwsu1t on the Nsh of 

### other organics preHftt in the 

### s.,ed a_spMre, the conc...trltions of 111 thl 1dsorINb1. Of"IIRics present. the _ient re1athe "'-ridity, the siIIIlPling rite for the organics 

### prwsent and the

# s."ng tille. 12. Cil1culate concentration. C

# <..-). of toluene in the air s,..led:

where: t". 

### length of s..,

# 'ng period (Min) K • uptake constant (CIt* to1uenelain). tGTE: The upuke constant .st be k

..... accurately (either be supplied by the**~l.r** 

### _nuflcturer or dlltenriMd by 

### the 

### user by c.liwation with standard**toluene-"~-a'r** 

### ",btures [5)). K 

### can be 

### "ti_ted f,... 

### the dtffus'on coefficient. 

### 0 (an2/1ti n), the cross-sectiON1 

### area. A (C112). and the diffusion pitlllength. L (aI), of the 

### s..ler:

EVAllMTlON OF fIEnII): Precisions and bilses listed in the _thod _,.. det.",'Md by analyzing generated 

### a"phlres COftuining various contentrations of toluene at 

### a r..... of ,..idities and in the presence of 

### other volatile organics 

### [3]. GeneraUdconcentrations 

### were independently 

### verified. REFEIEIICES: [1] Criteria for a Reel. LndId SUndard

...Oc:cupatloul Eaposure to Toluene. U.S. Deparwnt of

....,th. Education. and

# ""'a,... Pub\. (NIOSH) 13-11023 (1913). (2) NIOSH/OSHA OccupatiOftll ",,'t

...idelines for Ctt.ic.l Hazards. U.S. 1lepartlllent of 

### Hulth Mel

.....n services. Publ. (..IOSH) 81-123 (1981). available as Stock 1P883-1S4609 fMII NTIS. Springfield. VA 22161. (3] Perkins. J. Bo. N. N. price. L. Eggenberger and J. A. Burkart. Evaluation of Passive Qrginic Vaporftonitors. available as P883-221028 f,... NTIS. Springfield. VA 22161 (1981).

8115/81 4000-3 NIOSH**~nual** of Analytical "tthods 

### C-17

### TOlM 

# I

[4) Rodriguez, S. T•• O. W. 

### GosseH_. andA. E
....lUIIS. 

## ....te
.....tton of 

### Dnorption Efftctenctes 1ft 

### the 3500 Organic V..-or**fItonitor,··~.** 

### !!!l. 

### !1m. Assoc.**~."** 43,569-574 (1982)• [5) Hull. R. D ••nd It. E. 

### cllst

..nt., Testing Protocols wit.. £vllutiOlt**Cr'ter'~** 1M 

### Perforwnce Specificltions 

### for Pusi

.. Slllplen

......tted 

### to AIHAJ (1984). [6] 

### Woebkenberg, M. l. UnpIIblisMd dltl 

### 0.). METHOD WRITTEN 8Y: 

### "'ry Lynn
.....

### enberg. NIOSHIDPSE.

B/15/81 

### C-18 HIOSH Manual of Analytlcal PIIthods

# Personal 

# or Area Monitoringfor Dibasic Esters and styrene in Air (includlnadimethyl glutarate, dimethyl succinate, dimethyl adipate) -,**-----,------~.~-** -------"'--- ,----_.



### Principle Air is drawn by a personal battery-operated pump through atwo-section charcoal tube. where DBE and styrene vapors are adsorbed. The chem'lcals are desorbed with carbon disulfide/acetone and analyzed by gas chromatography. 

### Safety Wear leather gloveSto avoid cuts when handling broken glass tubes. Handle carbon disulfide In the hood. Review MSDSs for carbon disulfide, DBE, styrene and acetone. Avoid chemical contact with skin. Carbon disulfide is extremely flammable. 

### Validation The method for DBE wasdeveloped and validated by AnalyticS, Inc., Richmond, Virginia. Desorption efficiency for each of the esters when they were spiked to charcoal tubes over the range of 0.05-0.23 mg was98-104%. DynamiC standards in air were sampled. taking 4-8 L of air sample at 300 cc/min for 13-26 minute periods. Recovery of each ester at a feed concentration of 4- 17 mg/m3 was excellent. averaging 101 % with a CV of 0.03 Breakthrough of DBE from the front section to the back section in the charcoal tubes did not occur even after six hours of sampling at 300 cc/minute (108 L of air}. At Cape Fear, desorption efficiencies averaging 82 0 /0 were observed when DBE at concentrations of 0.01-1.1 mg were spiked. Capillary column GC was used at Analyties, packed column GC at Cape Fear. The method is sim'llar to the validated OSHA method for styrene. 

### Analysis To have samples analyzed. contact Roche Analytlcs. Richmond. Va., 1-800-888-8061. 

### Materials • Alprla 

### 2 ,l\ir Sampler. 5-200 cc!min range. or eqldvalent
• Charu)al tubes, Lot 120, 100/50 mg. WIth plastlr sealing caps, SKC 226-01

• PlastIC tubing to connect pump to tube • Charcoal tube holder and clothing clips • Tube tip breaker • Bubble tube calibrator or equivalent electron'le calibrator • Cas chromatograph equipped with 6-foot x c-mch stainless steel column packed with 0.1 0'0 SP-1 000 on 80il 00 mesh Carbopack C (Supelco). plus a peak area'lntegrator* • Exhaust trunk over CC to carry awayCS 1 odor* • Carbon disulfide,

### CS~ *

• Styrene*

• Acetone* • DBE* • Developingvials with TEFLON!) lined septum

cap, SKC 226-02A +0 • Developingvibrator, SKC, with vial rack* • Charcoal tube scoring file, and charcoal pick* • Assorted pipets: 1. 2, 10

### mt. etc. * • Syringe and needle for CC injections, 10 IJI Hamilton* • Electrical tape
• Sampling pump battery charger 

### Solutions· Make up 100 ml of desorbing solution with 98 ml of carbon disulfide and 2 ml of acetone. Do this in the hood. Store in closed glassbottle.

•-ecesserv for on·slte analysiS 

### C-193.7 minutes 

### 47 7.5 160 78 psig 

### 200°C 

### 8 minutes 

### 4° Clminute 2200 C 16 minutes 

### 1 4 

### 30 

### pSlg 30 psig 

### 200°C Use this solution to make your

### DBE standards, too. Do not keep the standards for more than a few days because of the possibility of loss of solvent by evaporation. 

### Standards

### * DBE Make up DBE standards in CS2iacetone as follows: DBE has 

### a specific gravity of 1.09 

### glml. 1% DBE by volume (0.0109**mg/~I)** 

### 0.1 

### % (0.00109 mg/I-!/J 

### 0.01 % (0.00011 mgil-!I) 

### Styrene If styrene is present, make up standards containing both styrene and DBE by also adding 1**~'D,** 0.1 

### % and 0.01 % styrene to the DBE standards. 

### 1q6 styrene by volume 

### [0.0091 mg/I-!l) 0.1 00 (0.00091 mg/I-!I) 

### 0.01 % [0.00009 mgfllll 

### Sampler Preparation 1. Start with a fully charged pump battery. 

### 2. Break tips off both ends of a charcoal tube. 

### 3. Calibrate pump with tube attached by plastic tubing to take air sample at 

### 100-200 cc/minute. The arrow on the tube indicates the direction of air flow (toward the pump). If the air sample will be of 4-8 hours duration, use '" 100 cc.rnmute flow. If of shorter duration. 

### use r- 200 

### cc.rninute. 4. Record on Figure 1: pump brand and model number, pump serial number, calibration date. and sampling rate. It may be useful to put a sticker on the pump with its sampling rate and calibration date 

### Taking Air Sample 1. Turn on the pump. Note on Figure 1 the time you started it. Close the case Fasten the pump to the belt or pocket of the worker you will monitor. Run the plastic tubing up his (her) back and clip the charcoal tube holder to the collar in front so that it samples air from near the face. Fasten the plastic tubing to the back of the shirt so that it won't flop around and get in the way. 

### 2. Write down on Figure 

### 1 also the employee's name and job description specifics while he will wear the sampler. Also write down the average air temperature and barometric pres- •necessary for on-sue ana'vSIS 

### C-20 sure while the sample is being taken. Observe the employee and record spills, leaks, odors. ventilation, symptoms, etc At the end of the air sampling turn off the pump, note the time 

### 3. Measure the pump air flow rate again to make sure that it has not changed significantly. Write the flow rate on Figure 1 and average the before and after flow rates. Record the average flow rate on Figure 1. 

### 4. Disconnect the charcoal tube and immediately cap the ends with the plastic caps furnished. Tag the tube with an identifying label or tape it to the paper with the information on employee name, etc. 

### Desorblnc the Charcoal* 1. With a thin wire charcoal pick, remove the glass wool holding the charcoal in the tube. Pour the larger section of charcoalmto one developing vial. After removing the foam plug pour the smaller section of charcoal Into another vial Add 

### 2 ml of desorbing solution to each vial (in the hood) and cap the vials immediately. Remember that the solution is extremely flammable, and stinky 

### 2. Label the vials to correspond with the samples and place them in the developing vibrator for 

### 30-60 minutes. 

### Cas Chromatocraph Calibration* 1. GCconditions are:

• helium carrier pressure
• initial oven temp.
• initial temp. hold time • oven temp. rate • final oven temp. • final temp hold time • range • attenuation
• hydrogen pressure • air pressure
• injector temp

. • detectortemp. 

### 250° C 

### 2. Inject 

### 1 microliter of 

### 1

### % standard 

### contairung 

### DBE and/or styrene. Approximate retention times (see also Figure 2) are: dimethyl succinate styrene dimethyl glutarate dimethyl adipateForthe DBE standard, the area ratios of DMS, DMG and DMA should be '" 17:66: 17. If retention times need to be increased or decreased, adjust the helium carrier flow. 

### 3. Also inject 1 III of 0.1 % standard. Areas of each of the peaks should be about 10% of what they were with the 1% standard. 4. Inject 1 111 of 0.01 

### % standard. Areas of each of the peaks should be about 10% of what they were with the 0.1 

### % standard. 

### Analysis of Samples 1. Inject 1 III of the solution desorbed from the largersection of charcoal. Compare the areas of the DBE and styrene peaks with the standard that is nearest in area. 

### 2. Inject 1 III of the solution desorbed from the smaller section of charcoal. In our experience there has never been any DBE or styrene in this backup section. even with 48 L of air sample. If there is more than 

### 25°0of what is found in the large section, the sample has been overloaded and should be discarded. 

### Calculations 1. Calculate the amount of DBE in the solution injected as follows: 

### 1

### a. Add together the areas of the DMS, DMG and DMA peaks in the sample. 

### 1b. Add together the same peaks in the DBE standard nearest 'In area. 1

### c. Divide the total DBE area in the sample by the total DBE area in the standard and multiply by the mg of DBE in one microliter of that standard. (See "Standards" section) 

### 1d. Example: 0.1 % DBE Standard 1 11\
- 0.001 09 mg DBE Areas: OMS 153.000 OMG 677,000 OMA 166,000 total 996.000 Sample from 41 .7 Lair Areas: OMS 200,000 DMG 397,000 DMA 176.000 total 773.000 773,000 

### x0.00109 = 0.00085 mg

### ~BE in 996,000 1 III sample Injected 

### 2. Do a similar calculation for styrene: Example: 0.1 % styrene standard 1 111=0.00091 mg styrene Styrene peak area 1,315,000 Sample from 41 

### .7 Lair Styrene peak area 638,000 638,000 x 0.00091 = 0.00044 mg styrene 1,315,000 In 1111 sample Injected 

### 3. Do similar calculations for the small sections of the charcoal tubes if any DBE or styrene are present. 4. Calculate the amounts of DBE and styrene found in each charcoal tube as follows: Multiply the mg of OBE found in the injections for each section by 2000. [There are 2000 microliters in the 

### 2 ml of desorbing solution.) Divide this number by 0.82 (the desorption efficiency measured in tests, "Validation" section). This will give you the mg of DBE and styrene collected on the charcoal tube. Add the amounts for the large and small sections together Example: DBE found in 1 III = 0.00085 mg Styrene found in 111\ = 0.00044 mg 000085 x 2000 2.07 mg OBE in charcoal 0.82 = tube large section (no DBE found in small section) 000044 x 2000 _ 1.07 mg styrene in char0.82 - coal tube large section (no styrene found in small section) 

### 5. Calculate the average DBE and styrene concentrations in the air sample as follows: 

### Sa. Calculate the volume of air sampled by multiplying average pump flow rate by minutes of air sampling. Example: 101 cc/rninute x 406 minutes = 41 ,006 cc air 5b. Convert average barometric pressure to mm Hg. Example: 29.70 inches

### x 25.4 = 754 mm Hg

### C-21 

# IFigure 1 Exposure Report Form for DBE and Styrene in Air Date NOTICE: USE 100 CCMIN FOR 4-8 HR SAMPLES. 200 CUMIN FOR SHORTER Location Area Name

_ Equipment Elevation SS#

_ Job assignments remarks, note when respirator IS worn

(V)

Small Section ____ cc3Ir
(Vel _--.--=:-_ ec air corrected 298 x

Large Section X - x 760 DBE analytical: Desorb eaen section in 2 ml of 2°0 acetone In

### es , Inject 1**~I** Standard Standard Used DMS Area

____ 00 DBE DMG Area

- mg DBE DIVIAArea in 1 III of Standard Total DBEArea Sampling method: One SKC 22601 charcoal tube, 10050 mg lot Pump Du Pont Alpha 2 Pump no Date pump last calibrated Pump rate cc.min before Final time

_ cCimll1 after Initial time

_ ec min avg Net time

_ Volume of air sample collected: average cc.rrun x minutes Average air temp, 0

### e [C) Average bar, press mm Hg (P) Volume corrected to standard V x 298 760 x C+ 273

Standard Large Small Total DBE Area In Large Section

Total DBE Area In Standard x mg DBE in 1 III Standard - mg DBE 111 1**~I** sample \ ------- mg DBE In 1 III of Large Section mg DBE In 1**~I** of Smal: Section total mg DBE In both SOlutions

____ mg DBE rr ______ mg DBE found mg DBE found x 1000,000 mg DBE m VC 100000(' = mg DBE X 082 Total mg DBE In both sotn. x 2000 _ mg DBE found In**char~oal** tube 0.82 x2000
DBE Concentration 111 ,,4.11

x mg Styrene In 1 III Standard - mg Styrene in 1 1-11 sample Stvrene Area Styrene analytical: Inject I**~I** Standard Used

____ 00 Styrene

____ mg Styrene In I IJI of Standard Styrene Area In Large SeCtion

Styrene Area in Standard Standard Large Section Sn'all Section

x _______ mg Styrene In 1 1-11 of Large Section

_______ mg Styrene 111 1 I!I of Small Section

_______ total mg Styrene In both solutions Total mg Styrene In both soln x 2000 _ mg Styrene found In charcoal tube 0.82

ppm Styrene ______mg Styrene found mgStyrene found x 24,450,000

_ ppm Styrene 104 

### ve x 2000 0,82 Styrene Concentration In Air
- mg Styrene x 24.450,000 104 REMARKS: Weather. wind direction, speed, employee comments, etc. ---------------- Sampled by Analyzed by

_ Date


### C·226.3 ppm styrene 

### or Sf. Calculate 

### average styrene concentration as ppm in air sample with this formula:

mg DBE found in charcoal tube 24,450,000 DBE 

### x . = ppm 

### avg. mol. wt. corr. air vol. of DBE Example:

2.07 mg DBE 

### x 24,450,000 = 7.9 ppm 159 40,143cc DBE 

### Sg. Calculate 

### average styrene concentration as ppm in air sample with this formula: mg styrene found In charcoal tube 24 450 000



### ------ x . . ' = ppm styrene molecular weight corr. air vol. of styrene Example: 1.07 mg styrene 24,450.000**--~----::..._-** 

### x 104 40,143cc 298 

### avg deg K Example: 41 006 

### x 754 

### x

, 760 298 40,143 cc air

= standard temp. 302 and pressure 

### Se. Calculate 

### average DBE concentration as rng/rn' in air sample with this formula mg DBE found in charcoal tube x 1,000.000 = mg DBE/m·

corrected air volume in cc Example: 2.07 mg DBE 1 000 000 51 6 rns/rn DBE

40,143 cc x 

### ivou. ,&' Sc. 

### Convertaverage temperature during sampling from degrees C to degrees K by adding 273. Example: 290 C 

### + 273 = 302 0 K 

### Sd. Correct air volume to standard conditions with this formula: calculated 

### x avg, bar. pres 

### x air volume 760



### Figure 2 GC Scan


### ( OMA 

# J _:7 ( OMG 

### --.-/ (**STYRE~E** l.-.--.-' OMS 

# .s' 18 

### 15 

### 12

# S 9 c 

## .- 6
3 

## o

100 

### 90 80 

### 70 60 

### 50 40 30 

### 20 10 

# o 1 III Solution of 1% DBE and 1% 

### Styrene 

### C-23

## • - I ! 

# f \ f I I
N-Kethyl-2-pyrrolidinone



### Matrix: Air 

### Tarre t 

### coneantratlont 51 ppe 

### (103**~/a')**



### 'rocedurel &&apIa. 

### are collected b1 draYin, &

### known 

### volu

.. 

### of air thr-ouab • charcoal tub,. 

# ....1.

.. are**de.or~.¥itb** 

### ".,

..th,leDI 

### chloride•••tbanol anet analy

..

### ct b)' p. c..**~t~** ..Ph1 yitb ana•• 

### ioalsation ctetector 

### (CC-'ID).

Air 

### vol

.... and 

## ".pUne nte 

### ,tudl.etl 10 liter. at 

### 0.2 Lpa.

Statu. of

..thode StoNa,

..tbod. This

..

### thod bal 

### been oDly pertially 

### tvaluated and 1. presented lOt 

### inforaation and trial u•••


## • 

# - II

Orpnle servlce lranch I

OSRA 

### Technical center Salt Lake 

### Cit7, Utah



### C-24 P.02... 4-

.......... <';\0

......

### k' , . t:::.. ,_, l>-1 ..... ' 1'1 J. ('4 P.o=:. 

# II**~p,N-n-9,** r x, 

### :5: 13 

## OSHA SLC**iECH~:CAL** 

## C7;**~HX** 

### NJ. 801 

### 524**~C51** 

## r.O; ,,,

1.1. laeklround 1.1.1. 81.tory of procedure 

### The OSHA 

### technical center hal 

### received .any requests for 

### a .a.p11na and analyt1cal proeedure for ••thyl pyrro11dlnone. Charcoal tube .ampl1n, end de.orption with 1 

### at carbOD di.ulfide va. tried ift1t!ally, but the desorpt1on .fficiency avarac_d 

### 3%.7l. Oe••

### rptloa with 1 aL 9911 

### carbon dl.ulf14.:DMF had concentration 

### '.pendent 

### desorption ran,ln. 

### fro. 73.2 

### to 1'.4 for 

### concentration. ranrin, froa 2.066 

### to**1'.5~8.,.** 

### o.lorptloft 

### with 1 

### aL 9515

..**t~l.n.** 

### chlorid.,

..thanol 

### averared 9g.4l for 

### concentration. froe 

### 0.1033 to 

### 2.066 

# aa. Charcoal tube, had ,ood .tor.,e 

### aD4 retention .fficlencie•• A tar,et level of 51 ppa Val 

### eho.en as it 

### 1. half the 

### r.c.....d.d TVA TLV li,ted on "SDS**fro~** 

### .everal Maufaeturul. 1.1.2. Potential workplace expo.ura (Iaf. '.1.) Kethyl p,rrolld1noa. 1. 

### u,,, al 

### a .olveftt in

..ny 

### appltcatlon.. It 1. 

### u'"

.. a**.ol~nt** 

### to 

### facilitate tbe**fo~t1Oft** 

### of -.ny 

### cbealcal.. It i.**u.~** al • 

### •olv«ftt 

### tor
..**~j~** 

### axtraction. 

### 1n eraek!n, 011. 

### and 1n 

### further**pet~ochealeal** 

### reaction.. It i. 

### v••d a. a MCltua 

### for pol,..rtaatioD, 

### and u ••olvent for**fIDi~"** 

### pol,..t.. It 

### 1. 

### u••d In .trippinl pottlh1

,••in. an4 

### .po.i•••. 1.1.3. 

### Toxic Iffect. (this .ectlon 

### is for 

### inforaatlon 

### purpo.e. and thould Dot
.. 

### taken IS 

### the 

### ba.t, for 

### OSHA pollcy.)(ltf. '.Z.) .ethyl 

### pynoli.inone 1n 

### ratt 

### had a tDLo 

### of 

### 7500 

### ./ke tot .kln 

### expo_un .. a LD of 3564

..

### /q, with ¥allbt 

### 10•• and body t••

### ,.ri9ure 

### d.er••••• noted in the 

### Ivt"Yhora. In**h~a".,** 

### ..thyl wrrolldlnone 

### h an lnhut n 

### eya., .kin aDd INeOU

..bruu. 

## rrol..,.. expolura "1 cau•• 

### headache, NU.... VOlll

### ti1\l and dhdnelS. 

### eoapound:

1**1~:16** 

### 801 !24 4081 p.e! 

### C-25

### • JAN-n-92 FRI :::**1~** 

## OSHA SLC TECHN1ChL C1R**FH~ ~J.**  

### 8Ql 524**~Cal** 

### - U.:. t



### SynonY•• 1**l-Metbyl-2-py~rolidlnon** 

### •• I-Methyl-'-pyrrolidinone, NHPI 

### Methyl 

### pyrrolidone; H-Pyrol "ol.cular 

### vat.ht: 99.13 Denslty, 

### 1.033 fralzinc poiDt' 

### -24'C 

### 1011ina pointl 

### 202'C Fla.h pointl 

### "'C (204") (open cup) Colors**colo~le.s** 

### liquid OdorJ .ild .mine-llkl 

### "olecular for.ulal C 519NO CAS: 872-'0-4 ItaSI RTSCS. 

### 11139 

### '4451 (VY"90000? 1.2. Ll.1t 

### dlflnin. par••eters 1.2.1. 

### The**det.~tion** 

### liMit 

### of the analytical 

### procedure 1. 4 ftC 

### wlth a 

### 1**~L** 

### injection volume. 

### Thi. 1. the
••alleat ••

### ount which 

### could be**d~t.cted** 

### uDder 

### nor••l 

### oper.tin. conditions. 1.2.2. 

### The ovu.ll detection Halt 18 0.1 'pll b

..

### ed on • 

### 10 liter air 

### volu... (All 

### ppa**a~unt.** in 

### thia .tudy 

### Ire based on a 10 L air 

### volume.) 1.3. Advent

.... 

### 1.3.1. Tbe ••mpling ptocedure t. 

### eonyenient. 1.3.2. 

### The analytical 

### method I, reproducible and .endtive. 1.3.3. R.analy_i. of .amples S. 

### po.slble. 

### 1.3.4. It
..y 

### be po.,ible to analyce other co.pound, at the •••• tillle.**1.3.~.** 

### Interferences**~y** 

### be avoided by proplr ••**l.ct~on** 

### of colu.n**.n~** 

### GC plrameterl.



### C-26

### FA}, t\S, 

### 4"" '. "", ,,-, r:.:. ... A 1.;.), ,",

# l

Due to the**voi.t1lit~** ot the meth)':x.ene chloride iu the 

### desorbina solvent, it

.., be DICI••lry 

### to have. fan blovinc on the instrument, in order to have consi.tent lnjettlon., vben 

### ul1n. an auto.aapler. 2.**Sa~pl1R1** 

### procedure 2.1. Apparatl.l. 2.1.1. A calibrated**"~Ional** 1 ••

### pI1nl pump. the flow of which c.n be detarained vithin + 

### 51 

### at the 

### reco...nded flov. 

### 2.1.2. Chareoal tubes, lot 120. cantatnina 100

.. 

### ad ••rb1nc .eetlon 

### with a 50

.. backup ••ction leparated**~y** • 

### 2

.. portioD of urethane foam, with 

### a .tlaniaed .1al. wool 

### plUi before the ad.orbi", .ection and a 

### 3

.. plul of urethane faa. at 

### the back of the backup

..etlon. Th. eD4h are 

## ne.a

...led 

### and the 

### ,la1. tub. contalnin. tbe ad.orbant 

### S. ? 

### c. 

### lon,. with a 

### 6
.. 

### O.D. and 

### 4 .m 1.0'1 

### IKe tubes or 

### equi.al.nt. • 

### 2.2. Sampllnc technique 

### 2.2.1. Open tbe 

### end. 

### of the charco.l tube.**i.~.dt.t.ly** before

...plinc. 

### 2.1.1. Connect the**ch.~coal** 

### tuba to 

### the ••**~pllnl** 

### puap with flexible tubin,.**2.~.3.** 

### 'lace the tube, in a vertical po.ition to 

### .inl.t•• chenn.line. vith tbe

...ller ••ction tovard' tha pUilp. 

### 2.2.6. A1r MiDI •..,led 

### ,houl. ftOt 

### pa.. 

### thl'O\&lh aJ11 

### ho

.. Dr tublna before**.~t.l'lft1** 

### tb. charcoal tube. 

### 2.2.5. s.al the charcoal tube vith pl••tic c.p.· 1

....i.t.l' after

...

### pline. ...1 .ach .ampl. 

### lencthwl•• vith 

### OSIA 'ora-Zl

...11ne tape. 

### 2.2.6. V1tb .ach bateh of 

### .a.plel. lubelt at le••t 

### one blank tube fro. the

.... lot used for

...pl••. Thi. tube ahould be 

### subjected to exactly the ••**~e** 

### handlinl 

### al the •••

### ple. (break 

### endl, ••

### al. , transport) except that no .1r 1••

### rawn thrOUJh 

### It. 2.2.7. Transport the**.~plel** 

### (and corre.pondlnl paperwork) to the lab for analys1•. 

### C-27 

# -

•

-I!

, I

J I. - 1 7 - ? F' P 1I· I

....... - .1-

-

_ tv-.4

.. ' .l. 1. : b- l k M • Ii:- '- MOM 1 N 

# I

JAN-P-92 FRI 15: 14 

## OSHA SLC TECHNICAL CiR FAX NO. SOl 524 4J5i

2.2.8. Bulk••",baitted for an.ly.i. au.t be ehipped in , 

### .ep.rate aail1nc cont.iner from 

### other •••**~1** 

### ••. 2.3. Desorption efficiency**Sl~** 

### tube••ere 11.ul••piked at ••ch**lo&di~** 

### of 0.103, 0.517, 1.03, &ftd 

### 2.07

..taL
..

### thyl 

### p,yrrolidinon.. The, vere alloved to equilibrate**~eI'ntlht** 

### at 1:00II 

### c ••perature. They ver. 

### openad, .aCh ••

### etion ,lac" into a ._para,e 2 aL vial, 

### •••••••4 -". 1 aL .f**,~.** ••**o.~I** ....lution. dftoorhnd**fn~** 30 .1nut•• v1tit 

### oceaaional .hakil\l, and ver. analyzed by CC-fID. the 

### ovu'all a"era,. vu 99." X.

### ('table 1

### >



## ... 

# TUM'

1 2 

### 3 4 5 6 

### Tabl. 1 De.orption zffielency 

### i lecoyerecs 0.103 ., 0.'11 III 

### 1.03

.. 2.07

... 

### 99.9 

## '9.S 100 100 M•• 

### 100 96.9 

### 99.6**98.~** 

# ".8 100 99.6 99.1 100 100 99.7 98.2 99.' 

### 99.G 100 

### ".0 

# "

# .. 99.3 99.7 99.0 

### 99.8 99.3 

### 99.7



### C-28 overall 

### .ver... 99.4 

### .tandard 

### devtation 0.73'

2.4. 

### aatentlon efUe1eney SlX tubel 

### .ere liquid 

### .piked with 2.07

.. ('1.0 

# ,,.>

..thyl pyrrolldiaon., al1ewed to 

### equilibrate overbl.ht, an. had 

### 10 liter. hUMi. 

### air (91t 

### II) pulled 

### throuch them. Th.y 

### .an 

### opened, 'e.orbed 

### an' andy.eel by 

### GC-rtD. Ttl.**ret~tlon** efficiency 

### a.arac" ".6%. There 

### v•• 

### no ••thyl pyrro1141none found on the backUp 

### portions 

### of the tubas. (Table 2)

4



### eet**~24** 41111**P.P~**... ... _ -J'...

......... t· • • , '.- ,....., .A...'. I .I.- I .. 

# I
OSHA SLC TECHNICAL eTR FAX NS. eOl**S2~** 

## 408:

Table 2 

### aetention !fflc1ency
Tube • 

### %

### Recovered t Itecovered Total 'A' 'I'
1 

### 99.9 0.0 99.9 2 97.7 

### 0.0 97.7 3 

### 98.9 0.0 98.9 4 

### 99.9 

### 0.0 99.9 5 101 

### 0.0 

### 101 6 100 

### 0.0 

### 100 avera,. 99.6 

# 2.'. Stor.,. Tub•• vere .piked vith 2.07

.. (Sl.0 ppe> ..th,l 

### pyrrolidiDOne and 

## Itor" at rooe t

..

## peraturl until opened and analyzed. The 

### ncoveri

....er.,.d 99.3 I 

### for the l' 

### day. 

### Itored.(Tabl. 3)

- T.ble 3 Stor.,. Study 

# ..

2.6.**r~.ch1on** Day
7 7 7 

### 15 15 

### 15 

### %Ilecoyued 

### 101

97.0 

# ".9 100 101 101



### !be ,reellion va. calculated ullft1 tb,**a~** 

### .. COuntl**fro~** 

### ai. injection. of 

### each .,an4ard at 

### eoncentrationa of 

### 0.103, 0.517, 1.03, and 2.07

..

# '.L

..thyl ,yrroltdinone in 

### the**.e.orbt~** 

### .olvent. The pooled coefficient of veriation va. 

### O.OO731.(Tabl. ')

C-29

l " II
- 1 7 _ a :'"**~.** l

### JAN-r7-S2 Fitl 15:

# is**F~X** 

## NO. SCi**S2~ ~061**  

## F.:: ." 

# I

Table J. Pnchlon Study 

### Injection

NWllber 0.103 lII/lDL 0.517 q/IlL 1.03 III/ilL 2.07 q/IIlL 

### 1 31014 147390 286310 568130 2 

### 31413 147880 

### 283730 '661'0 3 

### 31606 146470 286010 '71550 4 31033 147830 

### 288630 572910 

# , 31339 147000 288270 

## ",UO 6 31196 145030 

### 282800 574330 Averal' 31267 146933 285958 

### 569852 Standard Deviation 2)0 

### 1012 2347 3591 CV 

### 0.00136 0.00730 0.00821 O.OO6!lO 'ooled CV 

### 0.00131



# .. • vberet CV (Coefficient of Vart.tio") ••taDfard ••"latlon avera.e fooled I 

### .1(CV1)'Z • 

## 12(CV2S'2 • A3(CVS)'! • A4(CVl)-}

CV • 1\ I
--------------------------------------------- \ I 

### A1 • A' • A3 • A4

't 

### 4(1),A(2),A(3),A(4) •• of injections at ••cb 

### level CVl,CV2,CV3,CV4 • Coefficients at .ach level 2.7. Air yolu.. and .ampling rate atudied 2.7.1. The atr**volu~e** 

### atudied ia 10 lttera. 2.7.2. The .ampItnl rate studied 1. 0.2 litera per lIinute. 

## 2.'. Interference. Su.pected 1aterference, should b. l!.ted on ...ple ••ta .h••

## u.

C-30
J A**t~** - \ 7 - 9 2 F R 1 

### p,ee

### . JfLL.j-P-92**~Ri** 

### 15:15 

## OSHA SLC**TECH~;CAL** 

## erR FAX NO. BOl 524 4021 r 

# I L



### • 2.9. Satety 

### precautions 2.9.1. Samplin. eGui,.ent .hould be placed on an**.~ployee** 

### in a

..nner 

### that do•• not interfere vith work**p.rfor~.nt.** 

### or .afety. 2.9.2. Safety .1••••••hould be Yorn 

### at all tim••. 

### 2.9.3. 'ollov all ••fety praetiees 

### that apply 

### to 

### the workplace 

### be1nc •••

### pled. 

### 3. Analytical ••thod 

### 3.1. .pparatull 3.1.1. Ca. chroMetorr.ph 

### equlp,.d with. 

### 11.-. ionis.tion detector. • .. 5190 

### va. u••d 

### in thl• •tudy. 

### GC coluan capabl. 01

....r.tine the 

### an.1ft. and an internal 

### .tandard fro. aD1 interf.rence,. The 

### eoluan 

### uoed in**thi~ .t.~y** **Y.~** 

### a 60

..tlr**DI-V.~** 

### Yith 

### 0.5 u 

### d.l., 

### 0.32

.. I.D. 3.1.3. An 

### electroftic late,rator 

### or**.~** 

### other .uitable a.thod of 

### .a.urSftI peak 

### ere••. 

### 3.1.4. 'wo ail111iter vial. with teflon-lined cap•• 3.1.5. A 10**~L** 

### Iyrin.e or other con••nient .1z. for .aapl. injection. 3.1.6.**Pl~et.** 

### for dSspen.ln. the**'e.orbl~** 

### lolutton. 

### the Gleneo 1 .L d11penslc va. u••d 1ft thl• ••thocl. 

### 3.1.7.**Vol~tric** 

### flasks

- 5 

### at and other eoftvenient .lze. for preparinl It.ndard•• 3.2

.....nu 

### 3.2.1. Purified GC Irade nitroren, hydro.en, and aSr.

3.2.3. Methylene chlotid., IPte ,rade 3.2.4. Methanol, BPLC 

### .rad. 3.2.5. n-Iexanol. l.agent 

### Irad., u.e' a. the 

### internal .tandard 7 

# -

l e 'I _ , '? ;'(:, -, F F' I 

# -**_._~-** ....

# _----
OSHA SLC iECHNl:AL C;R**FA~** 

## N:. Sal 524 4C81**Th~ ~~~nrh1nr** **ftn1~rinA** 

### il**J~i~** 

# ..**'by~en, r"l~ri~~t~~fh~nn'**  

### vi'h 

### 0.1. 

### uL/mL**n-h'~RPul** 

### internal etandard. 3.3. Sample preparation 3.3.1. Sample tube. are opened and the front and back lection 

### of ••eh tube art placed 1n .eparate 2 aL 

### vi,h. 3.3.2. IIch**le~tion** 

### 1. de.orbed with 1 aL of the 

### d••orblna 

### .olytion of 

## ",5 ••thylene**~hlor14.:** 

### ..thanol with 

### 0.25**~L/.L** 

### n-hexanol internal ,tandard. 3.3.3. 

### The vial, 

### ar•••aled i

...

### diately and allowed to de.orb for 30 

### einute. with 

### occa.ional ahakin,. 

### 3.4. Standard 

### preparation 

### 3.4.1. Standard, are prepared 

### by dilutlft1 a 

### knovn Quantity 

### of

..thyl 

### pyrro114inofte with the de.orblna 

### solution. A Itandard of 1**~L'aL** 

### .ethyl 

### pyrro11d1none in 

### the 

### de.orbin••olution 1a 1033**~~~.** 

# . 3.4.2. At 

### l.a.t tvo leparate 

### stlndard. 

### et the ealibration level .hould be 

### .ade. 3•••3. A 

### third analytical atandard .hould be 

### prepare. at a hl.her concentration to check the lin.arity of 

### the detection. Por this stud, tvo .tandard. 

### at 1 

### uL/aL (1'0'3

../aL) and 

### on••tandard at 4**~L/~L** 

### (4.1)2 er/.L) .ethyl pyrrolidlnone 

### vera used. 3.5. 

### Analyd. 3.5.1. 

### Gas chroaatolraph condition•• Flov 

### rates**(~L/.ln.)** Injoctor1 200 

### Detectora 225 COlu.nl 

### aO·-lm!n 10·'.1n-160· 10

2 30 350 

### 1 "L ••e 'l,un 1**Rlt~v** 

### ••n(••ke-ur)1 

### Brdroc.n(carrier): Iydrolen(detector): Airl 

### InjectiDn dte: 

### Chroa.to.rall: 3.5.2. ..ak ar••• 

### are _e.lured 

### by an intelrator 

### or other lui

### table m.ans.

8 

### C-32
Tto**~l** - 1 7 -**~::** F' I el?ll '524 40131 P • 1 etnOllt DlIJ Imill11

### om ;rn 

# l

I ; ,,.. '1' ,"I,,,,

_



### 3.7.4. The above 

### equation. can be 

### con.olidated to 

### form the follovina**for~ul..** To 

### calculate the 

### ppw. of 

### analytl in the 

### campla baled on a 1"**'1t~r** 

### air

••lIpl@1**~I/~L** 

### • concentration of 

### analyt. in 

### .ampl. or 

### standard 24.45

- Holar**.ol~e** (litare/aole) 

### at 25 ·C 

### and 760 all 

## Ia. MV

_ Molecular vallht (1/ao1e) 

### DV • Desorption 

### volu•• 10 L • 10 liter air 

### .a.pla DE
- Desorption efficiency 

### 3.7.5. Thi. calculation 

### ts done 

### for .ach .action 

### of the 

### •..,11n, tub. and the 

### re.ult. added tOlether. 

### 3.8. Safety precautions 

### 3.'.1. All handliDI of .olvent••hould 

### be .one 

### 1n a hood. 3.8.2. 

### Avoid 'kin contact with all aolvent•• 

### 3.8.3. 

### Vear .afety 

### 11••••• at 

### all tta.a.
4. 

### aeco--andatlons for further atudy 

### Collectlon .tudie. nead to be 

### perforaed.



### 10 

### C-33 

# ..**~.** , !

## , JAH-l7-92 FRI 15:17 

## OSHA SLC TECHNICAL CiR FF.X Ne. 801 524 40Si

"'"" 

# = 0 

# ... I .I: 

# ... J


# .. • 

# " 

# - c:



## ... 0 0 c: 

# - 

# - u 

## • 

# - i rc;



## ....

# - ... 0 

# .. c 

# .... 

# j 

# .. l- e. 

# .. .... I I 

# :- e 

### ., 

# .,.. 

# l 

# .. .,.. 

# •

Fieur. 1. An 

### analytical**.tand.~d** 

### ot**1.0~S ~/wL**  ..

### th,l "rro11dinone 

### in the '.sorbin, solvent of 9Sz5 ..thyl.ne chlorid_,.eth.nol vith 

### n-haxanol internal .tandard.

.......
11F'. 1 4 

## OSHA SLC**TECH~:CAL** 

## eTR FAX NJ, 8:: 524**~C8\** 

### p, :**4,':~**



### 5.1. 

### Gr.yson. H., wKirk Oth

..r Encyclopedia of Chemical 

### Teehno10lY", Third Edition, 

### John W11ey , 

### Son, N.Y., 1981, 

### Vol. 19. p. 

### 616, and Vol. 20t 

### p.220. 5.2. 

### sv ••t, 

### D. t 

### ·"Il.try of 

### toxic Effecta of Chemical Sub.tanc••·, 1985-86 !ditlon, 

## u.s. Depart_ent of Health**and.~ft** 

### Servic••• 

### Public H ••lth Service, Center for 

### Dl••••• Control, NIOSH, 1987, Vol. 5. p. 

### 4223. 

### 5.3. Sax. N•• "Dana_roue 'ropertie. of Industrial Hatertal. n • 

### riftti adition, Van Mo.trand a.inhold 

### Co., N,v 

### fork, 1979. p. 1089.



### •



### 12 C-35 P. 1 4MFU-OppnA06-<l1 

### APPENDIX 0
FTlR RESULTS-AIR CONCENTRATIONS VS. 

### TIME

0-1

# AirConcentrations vs. Time RunNO.1

-

# alx Stripper 2000 I I

1500



# - i



# - !! I 

# .r 

# - I I. Methanol j 

# .. - I I ... Toluene 

# .= 1000 c: 

## 8 I 

# -' 

# - I I

.. Acetone c: 0 0 

# .. :.i 500

4 3.5 3 2.5 2 Time (hrs) 1.5 1 0.5 

### o**.**~** I I I I I I 

### I



## o
10.76airexchanges per hour

# l

o I V>



# -

## o 

# AirConcentration vs. Time RunNo.2 - SIXStripper
2000

# '~--------------------------l'

1500



# - i



# - 

# i**1~** L 

# I <; I ,_ Methanol

.. Toluene G> 

### I 

# ..- 

# -- I I

# * Acetone u 

# s 0 

## :i 500

4 3.5 3 2.5 2 Time (hrs) 1.5 1 0.5 

## o.........- -I I I J I I I
---- 

### I



### o
10.62airexchllng8lSper hour

# I



# -

# AirConcentrations vs. Time Run No.3 - BIXStripper 2000 I I

1500

........ 

# g

c

# 1~ 

# / • Methanol 0 4:1 

## g

... Toluene c CD 

# * Acetone o c 0 0 

# - :if 500

4 3.5 3 2.5 2 Time (hrs) 1.5 1 0.5 

## o I

...**~-** I 

## o I I I I I

10.61 airexchangesperhour

# I

o • 01



# -

## o I 0> 

# AirConcentrations

# vs. Time RunNo.4 - BIXSpray-On Stripper
2000

### I--------------------------~ I

1500



# - E g, g, 

# - I! ,8 1000 

# J <; I ,_ Methylene Chloride 

# i

.. Methanol 

# .. u c 0 0 

# .. < 500

4 3.5 3 2.5 2 Time (hrs) 1.5 1 0.5**O~I** I I I I I I I 

## o
10.57airexchangesper hour

### J

# AirConcentrations YS. 

# Time RunNo.5- BIXSpray-On Stripper
2000 I I

4 3,5 3 2,5 2 Time(hI'S) 1.5 1 0.5 0...,..."...... i t ( I ( ( I J



## o 1500



# - E Q. 

### S I) c: 

## :8 1000 

# I <; I 

# I- Methylene Chloride 

# g

.. Methanol c: G) u c: 0 0
500

10.57• exchanges per hour'



## o I



### ......



# --

# o I CD 

# AirConcentrationsvs. Time RunNO.6- SIXSpray-On Stripper 2000 , I

4 3.5 3 2.5 2 rune (hrs) 1.5 1 0.5**o~~** t I I 

## o I I I I I 1500 

## E 8: 

# - ! 

# 1 1000 

# J 

# '- I I_ Methylene Chloride

... Methanol 

## 3 c: 0 0 

# .. < SOD

10.58air

### exchangesper

### hour'



# ..

# Air Concentrationsvs. Time Run No.7 - Strypeeze
600 I \

500

'[ 400 

### S: 

# I J \. 

# I I- Methanol 

# j

_ .. _ .. Toluene 

## g 300

# I 

# I -. r-. · - ......- I 1* Methylene Chloride 

# a 

# f , '- B Acetone 

### o 200

100

4 3.5 3 2.5 2 Time (hrs) 1.5 1 0.5

### O~I I I I I I I 

## I o
10.56airexchanges perhour

# I

o I 

### co

-

# -

### o 

### •

...... 

### o 

# Air Concentrations vs. Time Run NO.8-

# strypeeze

4 3.5 3 2.5 2 Time(hrs) 1.5 0.5 

### o

## o 100 500 600



## E 400 

## 8: 

# - I ,r I \ 

# I I- Methanol 

# j

... IU
.... .. Toluene .: 300 _ . 

# I I 

# r**,r~~.** 

# I 

# 1::::nech'Oride o 

### ;l 200

10.54airexchanges perhous

# I



# ,..

# Air Concentrations vs. Time RunNo.9
- Strypeeze 600 i I

500

4 3.5 3 2.5 2 TIme (hrs) 1.5 0.5 

## oo 100 

# I 400 

# I 

# I_ Methanol 

# j I**~-,..** ... Toluene 

# i 300 

# r

-

# ......... I I* Methylene Chloride 

# I B Acetone 0 200

10.55 airexchangesperhouri



## o I


### .....


## .....



# -

## o • I\) 

# Air Concentration 

# vs. Time RunNo. 10- WoodFinisher's Pride

5 4.5 4 3.5 3 2.5 Time (hI'S) 2 1.5 0.5 

### o o 80 , ,

60



# - E 

# g c 

### :i as 

# 140 

# I I 

# I_NMPI

0 0 

# .. :.l IL 20

10.56 airexchanges PMhour

# I 

# J

# Air Concentration 

# vs. Time RunNo. 11 - WoodFinisher's Pride

5 4.5 4 3.5 3 2.5 Time (hfS) 2 1.5 0.5 

## o I - I I I i I I I I



## o 80 

## ,..--------------------------l'

60 

# - E e, 

# a c 

### :8 CIlI 

# I I § 40

# r I-NMPI 0 0 

## :<
20

10.54airexchanges per hour

# I

o I -" CJ) 

# J

## o , 

# Air Concentration 

# vs. Time RunNo. 12 -Wood Finisher's Pride 80

5 4.5 4 3.5 3 2.5 Time(hrs) 2 1.5 1 0.5 

## o r- \ I I I t I I J } I 

### o 60 

# - E a. a. 

# - c 

### :8 L'lI .:;; 40 

# j 

# I c 

### /- NMP

# I • o c: 0 0



## ... :.l Q. Z 20

10.57 airexchanges per hour

# I



# -

# Air Concentrations vs. Time Run No. 13- 3MSafestStripper



## o • C11 5 4.5

4 

# - E c. 3.5 c. 

# - c: 

## :8 3
lD 2.5 o s: 0 0


# ... 2 

# <



# ... 

# ! 1.5 

# I 1 0.5



## a -0.5 0 0.5
10.55airexchangesperhour

# l 1.5 2 2.5 3 3.5 Time(hrs) 4 4.5 5 5.5 6 

# I• Dibasic

### Esters

# I



# -

## o I -" 0> 

# Air Concentrations

# vs. Time Run

### No. 14- 3MSafestStripper
5 4.5

4


# -- K Q. 3.5 

# - c: 

# i 3 

### S 2.5 

## <3 2 

# j 1.5 

### w 

# j 1 

### C5 0.5 0 -0.5 0 0.5 (0.54 airexchangesperhour

# I 1.5 2 2.5 3 3.5 TIme(hrs) 4 4.5 5 5.5 

## s 

# I• Oibasic Esters

# I



# --

# AirConcentration VS. 

# Time Run No. 15 - 3MSafestStripper



## a •

...... 

# " 5 4.5

4 

# - E Co Co 3.5 

# - j 3 as .b c: 

## 8 2.5 c: 0 0 2 

## e 1.5**.~** 1 

## .! i5 0.5 0 -0.5 0 0.5 1
10.54airexchanges perhour

# l 1.5 2 2.5 3 3.5 Time (hrs) 4 4.5 5 5.5 6 

# I• Dibasic

### Esters

# I



# -

### o 

### , -" 

### en 

# Air Concentrations vs. Time Combined Plots for Runs 3, 6, 9, 12 & 15 2000 j I

4 3.5 3 2.5 2 Time (hrs) 1.5 1 0.5 

### o o

# ?~ • Methanol,Run 3 1500**~-** 

# I

... Toluene, Run3



# - E .. Acetone, Run3 

# g c B Methanol, Run6 

### :8 

## g 1000 -o- Math. Cl.. Run6

c GI -fs Methanol.Run 9 u c: 0 • Meth.CI., Run9 0



# ... 

# * Toluene, Run9
500**A~** .. Acetone, Run 9 B- NMP,Run12 

# * DBE,Run15



# -