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EMTIC CTM011  EMTIC CONDITIONAL TEST METHOD ă`X (#EPage 2 yx$xdddy spectroscopy. This confirming data must be available for review by the Administrator.  ?x  5.APPARATUS  ?  5.1 Sampling (see Figure 1). The sampling train consist of the following components:  ?`  5.1.1 Probe. Stainless steel, Pyrex glass, or Teflon tubing (as stack temperature permits), each equipped with a glass wool plug  ? to remove particulate matter. ( Note: Mention of trade names or specific products does not constitute endorsement by the Environmental Protection Agency)  ?  5.1.2 Sampling Line. Teflon, 6.4mm outside diameter, of sufficient length to connect probe to bag. Use a new unused piece for each series of bag samples that constitutes an emission test, and discard upon completion of the test.  ?  5.1.3 Quick Connects. Stainless steel male (2) and female (2), with ball checks (one pair without), located as shown in Figure1.  ?  5.1.4 Tedlar or Aluminized Mylar Bags. 100liter, to contain sample.  ?p  5.1.5 Bag Containers. Rigid leakproof containers for sample bags, with covering to protect contents from sunlight.  ?  5.1.6 Needle Valve. To adjust sample flow rate.  ?X  5.1.7 Pump. Leakfree, with minimum of 2liters/min capacity.  ?  5.1.8 Charcoal Tube. To prevent admission of halogenated organics to the atmosphere in the vicinity of samplers.  ?@  5.1.9 Flow Meter. For observing sample flow rate; capable of measuring a flow range from 0.10 to 1.00 liter/min.  ?!  5.1.10 Connecting Tubing. Teflon 6.4mm outside diameter, to assemble sampling train (Figure 1).  ?#  5.2 Sample Recovery. Teflon tubing, 6.4mm outside diameter, to connect bag to gas chromatograph sample loop is required for sample recovery. Use a new unused piece for each series of bag samples that constitutes an emission test and discard upon conclusion of analysis of those bags.  ?(  5.3 Analysis. The following equipment is needed: h)0*0*0*Ԍ ?  yx$dddy  ? EMTIC CTM011  EMTIC CONDITIONAL TEST METHOD ă`X (#EPage 3 yx$xdddy  ?   5.3.1 Gas Chromatograph. With FID, potentiometric strip chart recorder, and 1.0 to 2.0ml sampling loop in automatic sample valve. The chromatographic system shall be capable of producing a response to 0.1 ppm of the halogenated organic compound that is at least a great as the average noise level. (Response is measured from the average value of the baseline to the maximum of the waveform, while standard operating conditions are in use.)  ?`  5.3.2 Chromatographic Column. Stainless steel, 3.05 m by 3.2 mm containing 20 percent SP2100/0.1 percent Carbowax 1500 on 100/120 Supelcoport. The analyst may use other columns provided that the precision and accuracy of the analysis of standards are not impaired and information confirming that there is adequate resolution of the halogenated organic compound peak is available for review. Adequate resolution is defined as an area overlap of not more than 10 percent of the halogenated organic compound peak by an interferent peak. Calculation of area overlap is explained in Appendix E, Supplement A: "Determination of Adequate Chromatographic Peak Resolution."  ?  5.3.3 Flow Meters (2) . Rotameter type, 0 to 100ml/min capacity.  ?  5.3.4 Gas Regulators. For required gas cylinders.  ?  5.3.5 Thermometer. Accurate to 1$C, to measure temperature of heated sample loop at time of sample injection.  ?  5.3.6 Barometer. Accurate to 5 mm Hg, to measure atmospheric pressure around gas chromatograph during sample analysis.  ?X  5.3.7 Pump. Leakfree, with a minimum of 100ml/min capacity.  ?  5.3.8 Recorder. Strip chart type, optionally equipped with either disc or electronic integrator.  ?@  5.3.9 Planimeter. Optional, in place of disc or electronic integrator (Section 5.3.8), to measure chromatograph peak areas.  ?!  5.4 Calibration. Section 5.4.2 through 5.4.6 are for the optional procedure in Section 8.1.  ?#  5.4.1 Tubing. Teflon, 6.4mm outside diameter, separate pieces marked for each calibration.  ?H&  5.4.2 Tedlar or Aluminized Mylar Bags. 50liter capacity, with valve; separate bag marked for each calibration concentration. h)0*0*0*Ԍyx$dddy  ? EMTIC CTM011  EMTIC CONDITIONAL TEST METHOD ă`X (#EPage 4 yx$xdddy  ?   5.4.3 Syringes. One 25l and one 50l, gas tight, individually calibrated to dispense liquid halogenated organic solvent.  ?@  5.4.4 Dry Gas Meter with Temperature and Pressure Gauges. Accurate to +2 percent, to meter nitrogen in preparation of standard gas mixtures, calibrated at the flow rate used to prepare standards.  ?(  5.4.5 Midget Impinger/Hot Plate Assembly. To vaporize solvent.  ?  6.REAGENTS It is necessary that all reagents be of chromatographic grade.  ?  6.1 Analysis. The following are needed for analysis:  ?h  6.1.1 Helium Gas or Nitrogen Gas. Zero grade, for chromatographic carrier gas.  ?  6.1.2 Hydrogen Gas. Zero grade.  ?P  6.1.3 Oxygen Gas or Air. Zero grade, as required by the detector.  ?  6.2 Calibration. Use one of the following options: either Sections 6.2.1 and 6.2.2 or Section 6.2.3.  ?  6.2.1 Halogenated Organic Compound, 99 Mol Percent Pure. Certified by the manufacturer to contain a minimum of 99 Mol percent of the particular halogenated organic compound; for use in the preparation of standard gas mixtures as described in Section8.1  ?  6.2.2 Nitrogen Gas. Zero grade, for preparation of standard gas mixtures as described in Section 8.1.  ?  6.2.3 Cylinder Standards (3). Gas mixture standards (200, 100, and 50 ppm of the halogenated organic compound of interest, in nitrogen). The tester may use these cylinder standards to directly prepare a chromatograph calibration curve as described in Section 8.2.2, if the following conditions are met: (a) The manufacturer certifies the gas composition with an accuracy of +3percent or better (See Section 6.2.3.1). (b) the manufacturer recommends a maximum shelf life over which the gas concentration does not change by greater than +5 percent from the certified value. (c) The manufacturer affixes the date of gas cylinder preparation, certified concentration of the halogenated organic compound, and recommended maximum shelf life to the cylinder before shipment from the gas manufacturer to the buyer.h)0*0*0*Ԍyx$dddy  ? EMTIC CTM011  EMTIC CONDITIONAL TEST METHOD ă`X (#EPage 5 yx$xdddy  ?   6.2.3.1 Cylinder Standards Certification. The manufacturer shall certify the concentration of the halogenated organic compound in nitrogen in each cylinder by (a) directly analyzing each cylinder and (b) calibrating his analytical procedure on the day of cylinder analysis. To calibrate his analytical procedure, the manufacturer shall use, as a minimum, a threepoint calibration curve. It is recommended that the manufacturer maintain (1) a highconcentration calibration standard (between 200 and 400 ppm) to prepare his calibration curve by an appropriate dilution technique and (2) a lowconcentration calibration standard (between 50 and 100 ppm) to verify the dilution technique used. If the difference between the apparent concentration read from the calibration curve and the true concentration assigned to the low-concentration calibration standard exceeds 5 percent of the true concentration, the manufacturer shall determine the source of error and correct it, then repeat the threepoint calibration.  ?0  6.2.3.2 Verification of Manufacturer's Calibration Standards. Before using, the manufacturer shall verify each calibration standard by (a) comparing it to gas mixtures prepared (with 99Mol percent of the halogenated organic compounds) in accordance with the procedure described in Section 7.1 or by (b)having it analyzed by the National Institute of Standards and Technology, if such analysis is available. The agreement between the initially determined concentration value and verification concentration value must be within 5 percent. The manufacturer must reverify all calibration standards on a time interval consistent with the shelf life of the cylinder standards sold.  ?  6.2.4 Audit Cylinder Standards (2). Gas mixture standards with concentrations known only to the person supervising the analysis samples. The audit cylinder standards shall be identically prepared as those in Section 6.2.3 (the halogenated organic compounds of interest, in nitrogen). The concentrations of the audit cylinders should be : one lowconcentration cylinder in the range of 25 to 50 ppm, and one highconcentration cylinder in the range of 200 to 300 ppm. When available, audit cylinders may be obtain by contacting: Source Test Audit Coordinator (MD77B), Quality Assurance Division, Atmospheric Research and Exposure Assessment Laboratory, U.S. Environmental Protection Agency, Research Triangle Park, North Carolina 27711. The request for the audit cylinders must be made at least 30 days prior to the scheduled compliance sample analysis. h)0*0*0*Ԍyx$dddy  ? EMTIC CTM011  EMTIC CONDITIONAL TEST METHOD ă`X (#EPage 6 yx$xdddy  ?   7. PROCEDURE  ?  7.1 Sampling.  ?@  7.1.1 Assemble the sampling train as shown in Figure 1. Perform a bag leak check according to Section 8.3.2. Join the quick connects as illustrated, and determine that all connections between the bag and the probe are tight. Place the end of the probe at the centroid of the stack and start the pump with the needle valve adjusted to yield a flow that will more than half fill the bag in the specified sample period. After allowing sufficient time to purge the line several times, connect the vacuum line to the bag and evacuate the bag until the rotameter indicates no flow. At the time, direct the gas exiting the rotameter away from sampling personnel.  ?  7.1.2 Then reposition the sample and vacuum lines and begin the actual sampling, keeping the rate constant. At the end of the sample period, shut off the pump, disconnect the sample line from the bag, and disconnect the vacuum line from the bag container. Protect bag container from sunlight.  ?P  7.2 Sample Storage. Keep the sample bags out of direct sunlight and protect from heat. Perform the analysis within 1 day of sample collection for methylene chloride, ethylene dichloride, and trichlorotrifluoroethane, and within 2 days for perchloroethylene, trichloroethylene, 1,1,1trichloroethane, and carbon tretrachloride.  ?  7.3 Sample Recovery. With a new piece of Teflon tubing identified for that bag, connect a bag inlet valve to the gas chromatograph sample valve. Switch the valve to receive gas from the bag through the sample loop. Arrange the equipment so the sample gas passes from the sample valve to a 0 to 100ml/min rotameter with flow control valve followed by a charcoal tube and  Cx a 0 1in. H2O pressure gauge. The tester may maintain the sample flow either by a vacuum pump or container pressurization if the collection bag remains in the rigid container. After sample loop purging is ceased, allow the pressure gauge to return to zero before activating the gas sampling valve.  ?,#  7.4 Analysis. Set the column temperature to 100$C and the detector temperature to 225$C. When optimum hydrogen and oxygen flow rates have been determined, verify and maintain these flow rates during all chromatograph operations. Using zero helium or nitrogen as the carrier gas, establish a flow rate in the range consistent with the manufacturer's requirements for satisfactory detector operation. A flow rate of approximately 20 ml/min should produce adequate separations. Observe the base line (0*0*0*Ԍyx$dddy  ? EMTIC CTM011  EMTIC CONDITIONAL TEST METHOD ă`X (#EPage 7 yx$xdddy periodically and determine the noise level has stabilized and that baseline drift has ceased. Purge the sample loop for 30seconds at the rate of 100 ml/min, then activate the sample valve. Record the injection time (the position of the pen on the chart at the time of sample injection), the sample number, the sample loop temperature, the column temperature, carriers gas flow rate, chart speed, and the attenuator setting. Record the barometric pressure. From the chart, note the peak having the retention time corresponding to the halogenated organic compound, as determined in Section 8.2.1. Measure the halogenated organic  C compound peak area, Am, by use of a disc integrator, electronic  C integrator, or a planimeter. Record Am and the retention time. Repeat the injection at least tow times or until two consecutive values for the total area of the peak do not vary more than 5percent. Use the average value for these two total areas to compute the bag concentration.  ?p  7.5 Determination of Bag Water Vapor Content. Measure the ambient temperature and barometric pressure near the bag. From a water saturation vapor pressure table, determine and record the water vapor content of the bag as a decimal figure. (Assume the relative humidity to be 100 percent unless a lesser value is known.)  ?  8. PREPARATION OF STANDARD GAS MIXTURES, CALIBRATION, AND  ? QUALITY ASSURANCE.  ?@  8.1 Preparation of Standard Gas Mixtures. (Optional procedure delete if cylinder standards are used.) Assemble the apparatus shown in Figure 232. Check that all fittings are tight. Evacuate a 50liter Tedlar or aluminized Mylar Bag that has passed a leak check (described in Section 7.3.2) and meter in about 50 liters of nitrogen. Measure the barometric pressure, the relative pressure at the dry gas meter, and the temperature at the dry gas meter. Refer to Table 1. While the bag is filling, use the 50l syringe to inject through the septum on top of the impinger, the quantity required to yield a concentration of 200 ppm. In a like manner, use the 25l syringe to prepare bags having approximately 100 and 50ppm concentrations. To calculate the specific concentrations, refer to Section 9.1 (Tedlar bag gas mixture standards or methylene chloride, ethylene dichloride, and trichlorotrifluoroethane may be used for 1 day, trichloroethylene and 1,1,1trichloroethane for 2 days, and perchloroethylene and carbon tetrachloride for 10days from the date of preparation. (Caution: If the new gas mixture standard is a lower concentration than the previous gas mixture standard, contamination may be a problem when a bag is reused.) (0*0*0*Ԍyx$dddy  ? EMTIC CTM011  EMTIC CONDITIONAL TEST METHOD ă`X (#EPage 8 yx$xdddy  ?   8.2 Calibration.  ?  8.2.1 Determination of Halogenated Organic Compound Retention  ?x Time. (This section can be performed simultaneously with Section8.2.2.) Establish chromatograph conditions identical with those in Section 7.4 above. Determine proper attenuator position. Flush the sampling loop with zero helium or nitrogen and activate the sample valve. Record the injection time, the sample loop temperature, the column temperature, the carrier gas flow rate, the chart speed, and the attenuator setting. Record peaks and detector responses that occur in the absence of the halogenated organic. Maintain conditions (with the equipment plumbing arranged identically to Section 7.3), flush the sample loop for 30 seconds at the rate of 100 ml/min with one of the halogenated organic compound calibration mixtures, and activate the sample valve. Record the injection time. Select the peak that corresponds to the halogenated organic compound. Measure the distance on the chart from the injection time to the time at which the peak maximum occurs. This distance divided by the chart speed is defined as the halogenated organic compound peak retention time. Since it is possible that there will be other organics present in the sample, it is very important that positive identification of the halogenated organic compound peak be made.  ?  8.2.2 Preparation of Chromatograph Calibration Curve. Make a gas chromatographic measurement of each standard gas mixture (described in Section 6.2.3 or 8.1) using conditions identical with those listed in Sections 7.3 and 7.4. Flush the sampling loop for 30 second at the rate of 100 ml/min with one of the  C standard gas mixtures and activate the sample valve. Record Cc, the concentration of halogenated organic injected, the attenuator setting, chart speed, peak area, sample loop temperature, column temperature, carrier gas flow rate, and retention time. Record  C the laboratory pressure. Calculate Ac, the peak area multiplied by the attenuator setting. Repeat until two consecutive injection areas are within 5 percent, then plot the average of  C those two values versus Cc. When the other standard gas mixtures have been similarly analyzed and plotted, draw a straight line through the points derived by the least squares method. Perform calibration daily, or before and after each set of bag samples, whichever is more frequent.  ?$  8.3 Quality Assurance.  ?T&  8.3.1 Analysis Audit. Immediately after the preparation of the calibration curve and prior to the sample analyses, perform the analysis audit described in Appendix E, Supplement B: "Procedure for Field Auditing GC Analysis."(0*0*0*Ԍyx$ddd y  ? EMTIC CTM011  EMTIC CONDITIONAL TEST METHOD ă`X (#EPage 9 yx$xddd y  ?   8.3.2 Bag Leak Checks. While performance of this section is required subsequent to bag use, it is also advised that it be performed prior to bag use. After each use, make sure a bag did not develop leaks by connecting a water manometer and  C@ pressurizing the bag to 5 to 10 cm H2O (2 to 4 in. H2O). Allow to stand for 10 min. Any displacement in the water manometer indicates a leak. Also, check the rigid container for leaks in this manner. (Note: An alternative leak check method is to  Cd pressurize the bag to 5 to 10 cm H2O 2 to 4 in.H2O) and allow to stand overnight. A deflated bag indicates a leak.) For each sample bag in its rigid container, place a rotameter in line between the bag and the pump inlet. Evacuate the bag. Failure of the rotameter to register zero flow when the bag appears to be empty indicates a leak.  ?  9. CALCULATIONS  ?p 9.1 Optional Procedures Standards Concentrations. Calculate  C8 each halogenated organic standard concentration (Cc in ppm) prepared in accordance with Section 8.1 as follows: k!#xDdddddc ddw x `k Eq. 1XRC_c~=~{{24.055~x~10^3}~{{B~D} over M}} over{{V_m~Y~}{293 over T_m}~{P_m over 760}}!Cxxc+(224".055Zx*10xx3\!B!DMDMVxxWmY | >293WaTxx-m |ggPxx3ma760k$(#(#(#(#x!!'#$ X` hp x (#%'0*,.8135@8:aSxx-wbGa)y$(#(#l (#(#!A'#$ where:  Ct @;` Cc = Concentration of the halogenated organic indicated by ` ` P P the gas chromatograph, ppm.  C @D` Pr =P P Reference pressure, the laboratory pressure recorded during calibration, mm Hg.(#P  C, @D` Tr =P P Sample loop temperature at the time of analysis, $K.(#P  C @O` Pi =P P Laboratory pressure at time of analysis, mm Hg.(#P  CT @D` Tr =P P Reference temperature, the sample loop temperature recorded during calibration, $K.(#P  C @` Swb =P P Water vapor content of the bag sample, fraction.(#P X` P hp x (#%'0*,.8135@8: