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OSHA Method 61: Phosgene

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OSHA Method 61: Phosgene PHOSGENE - (Organic Method #61) Page 1 of 20 U.S. Department of Labor Occupational Safety & Health Administration www.osha.gov Search Advanced Search | A Technical Links > Sampling & Analytical Methods > Index PHOSGENE Method no.: 61 Matrix: Air Target concentration: 100 ppb (0.4 mg/m3) (OSHA PEL) Procedure: Air samples are collected by drawing known volumes of air through sampling tubes containing XAD-2 adsorbent which has been coated with 2­ (hydroxymethyl)piperidine. The samples are desorbed with toluene and then analyzed by gas chromatography using a nitrogen selective detector. Recommended air volume and sampling rate: 240 L at 1 L/min Reliable quantitation limit: 3.5 ppb (0.014 mg/m3) Standard error of estimate at the target concentration: 6.7% (Section 4.7.) Status of method: Evaluated method. This method has been subjected to the established evaluation procedures of the Organic Methods Evaluation Branch. Date: August 1986 Chemist: Warren Hendricks Organic Methods Evaluation Branch OSHA Analytical Laboratory Salt Lake City, Utah 1. General Discussion 1.1. Background 1.1.1. History http://www.osha.gov/dts/sltc/methods/organic/org061/org061.html 7/7/2008 PHOSGENE - (Organic Method #61) Page 2 of 20 The procedures that have been used by OSHA to monitor occupational exposure to phosgene include detector tubes, monitoring dosimeters and infrared gas analyzers. None of these procedures have proven to be completely adequate for use by OSHA. These methods lack either the desired precision and accuracy or they are awkward and inconvenient for field use. This procedure was developed after it was found that phosgene would react quantitatively with 2-(hydroxymethyl)piperidine (2-HMP) to form a stable derivative, 1-aza-8-oxabicyclo[4.3.0.]inonan-9-one. The proposed derivatization reaction is presented below. The structure of the derivative has been confirmed by mass spectrometry. Phosgene 2-HMP Derivative XAD-2 adsorbent coated with 2-HMP is used in the OSHA method for acrolein and formaldehyde (Method 52) (Ref. 5.1.). This procedure was successfully evaluated using the same adsorbent tube that is used in Method 52, thereby extending its use to a third analyte. 1.1.2. Toxic effects (This section is for information only and should not be taken as the basis of OSHA policy.) Phosgene gas is a severe eye and respiratory irritant. The lowest concentration that will cause immediate throat irritation is 3 ppm. A level of 4 ppm will cause immediate eye irritation, 4.8 ppm causes coughing and brief exposure to 50 ppm may be fatal. Symptoms of moderate exposure include a dryness or a burning sensation in the throat, vomiting, chest pain and difficulty in breathing. Inhalation of a sufficient quantity of phosgene causes pulmonary edema which may be characterized by a delay in the onset of symptoms of up to 72 h. The length of the delay in the onset of symptoms depends on the severity of the exposure. The pulmonary edema may progress to pneumonia which may result in cardiac failure. (Ref. 5.2.) Splashes of liquid phosgene on the skin or in the eye may produce severe tissue damage (Ref. 5.2.). The odor threshold for phosgene is about 0.5 to 1 ppm. This level will vary with the individual and is usually higher following exposure because of olfactory fatigue. The odor of phosgene at 0.5 ppm has been described as pleasant and similar to new-mown hay or cut-green corn. At higher levels, the odor may be strong, stifling and unpleasant. (Ref. 5.3.) 1.1.3. Workplace exposure Most phosgene is used to manufacture other chemicals in the same plant in http://www.osha.gov/dts/sltc/methods/organic/org061/org061.html 7/7/2008 PHOSGENE - (Organic Method #61) Page 3 of 20 which it is produced. It is manufactured by the reaction of carbon monoxide and chlorine over activated charcoal. In 1981, the United States consumed almost a million metric tons. The primary user of phosgene is the polyurethane industry which consumes 85% of the total phosgene produced. The polycarbonate industry consumes about 6% and the remaining 9% is used in miscellaneous applications. Phosgene can be employed in a variety of metal recovery operations and in the production of chloroformates which are intermediates in the production of perfumes, herbicides, insecticides and pharmaceuticals. Phosgene also has numerous other minor uses and suggested uses. (Ref. 5.3.) In 1976, NIOSH estimated that 10,000 workers had potential occupational exposure to phosgene during its manufacture and use (Ref. 5.4.). Phosgene can be unintentionally produced when chlorinated hydrocarbons are subjected to heat or light. An example of this is the production of phosgene in the vicinity of a welding operation in a facility in which perchloroethylene is used. (Ref. 5.4.) 1.1.4. Physical properties (Ref. 5.3.) CAS no.: 75-44-5 molecular weight: 98.92 appearance: colorless gas melting point: -127.84°C boiling point at 1 atm: 7.48°C vapor pressure at 20°C: 1212 mm Hg vapor density (air = 1.0): 3.4 molecular structure: synonyms: carbonyl chloride; carbon oxychloride; chloroformyl chloride 1.2. Limit defining parameters (The analyte air concentrations listed throughout this method are based on an air volume of 240 L and a solvent desorption volume of 1.0 mL. Air concentrations listed in ppm are referenced to 25°C and 760 mm Hg. The analyte concentrations are listed as phosgene even though the derivative is the actual species analyzed.) 1.2.1. Detection limit of the analytical procedure The detection limit of the analytical procedure is 2.7 ng per injection. This is the amount of analyte which will give a peak whose height is sufficiently large to permit its visual detection in a sample chromatogram when it is compared to a blank sample chromatogram. (Section 4.1.) 1.2.2. Detection limit of the overall procedure The detection limit of the overall procedure is 3.4 µg per sample (3.5 ppb or 0.014 mg/m3). This is the amount of phosgene spiked on the sampling device which allows recovery of an amount of analyte equivalent to the detection limit of the analytical procedure. (Section 4.2.) 1.2.3. Reliable quantitation limit http://www.osha.gov/dts/sltc/methods/organic/org061/org061.html 7/7/2008 PHOSGENE - (Organic Method #61) Page 4 of 20 The reliable quantitation limit is 3.4 µg per sample (3.5 ppb or 0.014 mg/m3). This is the smallest amount of analyte which can be quantitated within the requirements of a recovery of at least 75% and a precision (±1.96 SD) of ±25% or better. (Section 4.2.) The reliable quantitation limit and detection limits reported in the method are based upon optimization of the instrument for the smallest possible amount of analyte. When the target concentration of an analyte is exceptionally higher than these limits, they may not be attainable at the routine operating parameters. 1.2.4. Instrument response to the analyte The instrument response over the concentration range of 0.5 to 2 times the target concentration is linear. (Section 4.4.) 1.2.5. Recovery The recovery of phosgene from samples used in a 19-day storage test remained above 102% when the samples were stored at about 23°C. (Section 4.7.) The recovery of the analyte from the collection medium during storage must be 75% or greater. 1.2.6. Precision (analytical procedure) The pooled coefficient of variation obtained from replicate determinations of analytical standards at 0.5, 1 and 2 times the target concentration is 0.035. (Section 4.3.) 1.2.7. Precision (overall procedure) The precision at the 95% confidence level for the 19-day ambient temperature storage test is ±13%. (Section 4.7.) This includes an additional ±5% for sampling error. The overall procedure must provide results at the target concentration that are ±25% or better at the 95% confidence level. 1.2.8. Reproducibility Six samples, collected from a controlled test atmosphere, and a draft copy of this procedure were given to a chemist unassociated with this evaluation. The samples were analyzed after 1 day of storage at 23°C. No individual sample deviated from its theoretical value by more than the precision reported in Section 1.2.7. (Section 4.8.) 1.3. Advantage This sampling and analytical procedure provides a simple, convenient and precise means to monitor occupational exposure to phosgene. 1.4. Disadvantage http://www.osha.gov/dts/sltc/methods/organic/org061/org061.html 7/7/2008 PHOSGENE - (Organic Method #61) Page 5 of 20 The sampling tubes currently must be obtained from the Salt Lake City Analytical Laboratory (SLCAL). 2. Sampling Procedure 2.1. Apparatus 2.1.1. Samples are collected by use of a personal sampling pump that can be calibrated to within ±5% of the recommended flow rate with the sampling device in line. 2.1.2. Samples are collected on 4-mm i.d. × 6-mm o.d. × 11-cm long silane- treated glass tubes which are packed with a 75-mg backup section and a 150­ mg sampling section of pretreated XAD-2 adsorbent which has been coated with 2-HMP. The two sections of coated adsorbent are separated and retained with small plugs of silanized glass wool. Instructions for the pretreatment and the coating of XAD-2 adsorbent are given in Section 4.10. of this method. 2.1.3. Commercially available sampling tubes, marketed by Supelco for the collection of acrolein, while similar to those in this method, are not recommended by SLCAL for the collection of phosgene. These sampling tubes provided consistently lower results than SLCAL tubes when the same test atmosphere was sampled with both tubes.
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