Document GmLLQVJo3rjnG68bXvyVBvxeV

ENVIRONMENTAL HEALTH SURVEY REPORT January 23, 1978 PHENOL AREA/ MONITORING AT THE CHLORINATED SOLVENTS PLANT INTRODUCTION The collection and determination of phenol in air using silica gel adsorption tubes has been accomplished with much success (R.G. Melcher and J.S. Warren, I.H, Analytical Method Pile, Method #559 of ML AL 77-50520). Short term (10 minutes to 1 hour) as well as long term (4 to 8 hours) sampling is easily achieved with these tubes, even in highly humid air. Also, by using a mixed solvent composed of 10% methanol in ether by volume, high desorption efficiencies are obtained with a minimum of tailing problems in the analysis. This report includes both a recovery efficiency study and the results of air samples collected at various locations within the Solvents Plant. A linearity study of the analytical method was also conducted and found to be within acceptable limits. EXPERIMENTAL Standard Preparation: Stock solutions containing 38 and 19 milligrams of phenol per 100 ml. of solvent were prepared by injecting 35.5 and 17.8 microliters of the liquified compound into 100 ml. volumetric flasks and diluting to volume with a mixed solvent composed of 10% methanol in ether by volume. Work ing standards of 0.5, 1.5, 3.8 and 9.5 milligrams per 100 ml. solvent were prepared by pipetting appropriate amounts of the 38 milligram stock solution into 100 ml. volumetric flasks and diluting to volume with the mixed solvent. These standards were analyzed to check the linearity of the detector (See Graph 1). Analytical Parameters: A Hewlett-Packard,Model 5730 A, gas chromatograph equipped with a flame ionization detector was used for the analyses. Chromatographic conditions are as follow: DO 088917 OONFTDFNTTAt January 23, 1978 PHENOL AREAE!' MONITORING Page - 2 - Analytical Parameters: (continued) Column: 10* X 1/8" 8S 10% FFAP on 100/120 Mesh Gas chrom W-(AW) Temperatures: Oven - 200 C Isothermal Injector - 200 C Detector - 200 C Carrier Gas: Nitrogen at 35 ml/minute flow Range: X 10 Sample Size: 2 microliters Phenol Elution Time: 4.8 minutes Recovery Efficiencies: The phase equilibrium recovery method was used to study recovery efficiencies. It consists of injecting a known amount of a compound into a suitable solvent, adding a known amount of adsorbent, and allowing the mixture to come to equilibrium. The recovery efficiency is determined by dividing the amounts found by the amounts added. These tests were per formed on two section tubes containing 260/560 mg. of silica gel (Tek Labs Inc., catalog no. 226-15). Recovery of phenol was approximately 100% for all concentration levels tested (See Table I). The high results observed in several of the samples may be due to partial solvent loss during desorption. MONITORING PROCEDURES Collection of Samples: SP-1 personal air sampler pumps were used for collecting the samples. The silica gel tube was attached to the pump inlet via a 2 ft. piece of amber latex tubing (3/16" X 1/8"). All pumps were calibrated to operate at 150 ml/minute flow with a soap bubble meter. One, four, and eight hour samples were collected over a period of one week. Sample Preparation: Samples were desorbed by dumping the silica gel into 5 ml. of chilled mixed solvent and then shaking periodically for one hour. Analysis was performed by F.I.D. The peak height of the resulting trace was measured and the corresponding weight in milligrams read from a standard curve. F * /" t > h * * , ' ' - * p p 00 088918 CONFIOFNTTAI January 23, 1978 PHENOL AREAZf MONITORING Page - 3 - Sample Preparation: (continued) A volume correction was made since the calibration curve was based on mg/100 ml. of mixed solvent and samples were desorbed with only 5 ml, of mixed solvent. Corrected mg = C X (mg sample - mg blank) where: mg sample mg blank C = milligrams phenol found in sample = milligrams phenol found in blank = volume correction factor = 0.05 Calculations: Concentrations of phenol in the air sample are expressed as follows: (a) milligrams per cubic meter air mg/cu m air corrected mg X 100 (liter/cu m) air volume sampled (liter) (b) Parts per million by volume ppm(v) = mg/cu m X 6 A5 X 1MI x ^ ~*T-- MW P 298 where: P = pressure (mm Hg) of air sampled T = temperature (degrees C) of air sampled 24,45 = molar volume (liter/mole) at 25 C and 760 mm Hg MW molecular weight (g/mole) of phenol = 94.11 760 standard pressure (mm Hg) 298 = standard temperatures (degrees Kelvin) DO 088919 CONFTOFNTTAl January 23, 1978 PHENOL AREA? MONITORING Page - 4 RESULTS AND DISCUSSION The ppm phenol and the corresponding mg/cu m value are shown In Table II. Eight hour samples were only collected in the vinylidene process area since no phenol was detected in the majority of the one and four hour samples obtained In other areas of the plant. All samples indicated that the airborne concentrations of phenol at the Chlorinated Solvents Plant are well within the 5 ppm or 19 mg/cu m air exposure limit set by OSHA. L. R. Smith Industrial Hygienist Chlorinated Solvents Plant DO 0R8970 CONFTOFNTTAI GRAPH 1 : LINEARITY PLOT Peak H eight X 10" DO 0 R 8 9 ? ] CO NriDDNTTAI <avu `M i < ir j i Jh j u, i -.Hi DO 0 8 8 9 ? ? CO NFIDENTIAL r, 1 TABLE I PHENOL PHASE EQUILIBRIUM RECOVERY DATA FOR SILICA GEL TUBES DESORBED WITH DIETHYL ETHER CONCENTRATION: Sample # 1 Sample # 2 Sample # 3 Average 2 X TLV 100 100 101 100 TLV* 92 94 98 95 1/2 TLV 102 101 100 101 1/5 TLV 99 100 97 99 * TLV 19 milligrams DQW lulhAo! TABLE II 'RATION LEVELS AT THE CHLORINATED SOLVENTS PLANT - 1978 DO 0 8 8 9 7 3 CONFTDFNTTAl SAMPLE # 100 101 102 103 104 105 SAMPLING DATE 1/13/78 II 11 " 11 II SAMPLING TIME (HRS) 1.0 11 tl tl ir " MG/CU M N/D 0.26 0.44 N/D N/D N/D PPM PHENOL N/D 0.06 0.11 N/D N/D N/D 106 107 108 109 110 111 1/16/78 II rt it n n 4.0 ir n 11 rr rr N/D N/D N/D 1.08 N/D 0.10 N/D N/D N/D 0.27 N/D 0.03 112 113 114 115 116 117 1/19/78 IT ir ii n ii 8.0 11 tl 11 II II 0.39 0.12 0.04 0.02 0.02 trace ( 0.01) 0.09 0.03 0.01 0.01 0.01 0.01 NOTE: Wind out of the North at 10-15 mph on 1/13/78. Wind out of the South at 10 mph on 1/16/78. Wind out of Northwest at 10 mph on 1/19/78. N/D = None detected SAMPLE LOCATION: Control room New lab ^ Downwind C-94 Btms pump Old lab" Downwind of T-97 & 98 pumps ' Downwind of R-90 Control room Old lab v New lab w Downwind of C-94 Btms pump f Downwind of base of R-90 Downwind of T-97 & 98 pumps Downwind of T-97 & 98 pumps Downwind of T-94 pump Downwind of C-94 Btms pump Downwind of base of R-90 Downwind of tarpot pumps Downwind of T-95 pumps