EPA Method 310B Determination Of Residual Solvent Through Gas Chromatography
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F05A82A6D42741F9A8C534C69475006C |
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0.04 |
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14 |
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日期: |
1998-5-13 |
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1,METHOD 310B - DETERMINATION OF RESIDUAL SOLVENT THROUGH GAS,CHROMATOGRAPHY,1.0 SCOPE AND APPLICATION,ANALYTE CAS MATRIX METHOD,NUMBER SENSITIVITY,(5.5g sample,size),hexane 110-54-3 rubber .01 wt%,crumb,ethylidene 16219-75- rubber .001 wt%,norbornene 3 crumb,(ENB),1.1 Data Quality Objectives:,In the production of ethylene-propylene terpolymer crumb,rubber, the polymer is recovered from solution by flashing,off the solvent with steam and hot water. The resulting,water-crumb slurry is then pumped to the finishing units.,Certain amounts of solvent (hexane being the most commonly,used solvent) and diene monomer remain in the crumb. The,analyst uses the following procedure to determine those,amounts.,2.0 SUMMARY OF METHOD,2.1 The crumb rubber sample is dissolved in toluene to,which heptane has been added as an internal standard.,Acetone is then added to this solution to precipitate the,crumb, and the supernatant is analyzed for hexane and diene,by a gas chromatograph equipped with a flame ionization,detector (FID).,3.0 DEFINITIONS,3.1 Included in text as needed.,4.0 INTERFERENCES,4.1 None known.,4.2 Benzene, introduced as a contaminant in the toluene,solvent, elutes between methyl cyclopentane and,2,cyclohexane. However, the benzene peak is completely,resolved.,4.3 2,2-dimethyl pentane, a minor component of the hexane,used in our process, elutes just prior to methyl,cyclopentane. It is included as "hexane" in the,analysis whether it is integrated separately or,included in the methyl cyclopentane peak.,5.0 SAFETY,5.1 This procedure does not purport to address all of the,safety concerns associated with its use. It is the,responsibility of the user of this procedure to,establish appropriate safety and health practices and,determine the applicability of regulatory limitations,prior to use.,5.2 Chemicals used in this analysis are flammable and,hazardous (see specific toxicity information below).,Avoid contact with sources of ignition during sample,prep. All handling should be done beneath a hood.,Playtex or nitrile gloves recommended.,5.3 Hexane is toxic by ingestion and inhalation. Vapor,inhalation causes irritation of nasal and respiratory,passages, headache, dizziness, nausea, central nervous,system depression. Chronic overexposure can cause,severe nerve damage. May cause irritation on contact,with skin or eyes. May cause damage to kidneys.,5.3 ENB may be harmful by inhalation, ingestion, or skin,absorption. Vapor or mist is irritating to the eyes,mucous membranes, and upper respiratory tract. Causes,skin irritation.,5.4 Toluene is harmful or fatal if swallowed. Vapor,harmful if inhaled. Symptoms: headache, dizziness,hallucinations, distorted perceptions, changes in motor,activity, nausea, diarrhea, respiratory irritation,central nervous system depression, unconsciousness,liver, kidney and lung damage. Contact can cause,severe eye irritation. May cause skin irritation.,Causes irritation of eyes, nose, and throat.,5.5 Acetone, at high concentrations or prolonged,overexposure, may cause headache, dizziness, irritation,of eyes and respiratory tract, loss of strength, and,3,narcosis. Eye contact causes severe irritation; skin,contact may cause mild irritation. Concentrations of,20,000 ppm are immediately dangerous to life and,health.,5.6 Heptane is harmful if inhaled or swallowed. May be,harmful if absorbed through the skin. Vapor or mist is,irritating to the eyes, mucous membranes, and upper,respiratory tract. Prolonged or repeated exposure to,skin causes defatting and dermatitis.,5.7 The steam oven used to dry the polymer in this,procedure is set at 110o C. Wear leather gloves when,removing bottles from the oven.,6.0 EQUIPMENT AND SUPPLIES,6.1 4000-ml volumetric flask,6.2 100-ml volumetric pipette,6.3 1000-ml volumetric flask,6.4 8-oz. French Square sample bottles with plastic-lined,caps,6.5 Top-loading balance,6.6 Laboratory shaker,6.7 Laboratory oven set at 110E C (steam oven),6.8 Gas chromatograph, Hewlett-Packard 5890A, or,equivalent, interfaced with HP 7673A (or equivalent),autosampler (equipped with nanoliter adapter and,robotic arm), and HP 3396 series II or 3392A (or,equivalent) integrator/controller.,6.9 GC column, capillary type, 50m X 0.53mm, methyl,silicone, 5 micron film thickness, Quadrex, or,equivalent.,6.10 Computerized data acquisition system, such as CIS/CALS,6.11 Crimp-top sample vials and HP p/n 5181-1211 crimp caps.,6.12 Glass syringes, 5-ml, with "Luer-lock" fitting,4,6.13 Filters, PTFE, .45Fm pore size, Gelman Acrodisc or,equivalent, to fit on Luer-lock syringes (in 6.12,above).,7.0 REAGENTS AND STANDARDS,7.1 Reagent toluene, EM Science Omnisolv,PURITY CHECK:……
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