EPA Method 313B The Determination Of Residual Hydrocarbon In Solution
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ID： |
1C0E33E00DB04EACA6F77E15F7A9904E |
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文件大小(MB)： |
0.02 |
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页数： |
8 |
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文件格式： |
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日期： |
1998-5-13 |
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文本摘录（文本识别可能有误，但文件阅览显示及打印正常，pdf文件可进行文字搜索定位）：
1,METHOD 313B - THE DETERMINATION OF RESIDUAL HYDROCARBON IN SOLUTION,POLYMERS BY CAPILLARY GAS CHROMATOGRAPHY,1.0 SCOPE,1.1 This method is applicable to solution polymerized,polybutadiene (PBD).,1.2 This method quantitatively determines n-hexane in wet crumb,polymer at levels from 0.08 to 0.15% by weight.,1.3 This method may be extended to the determination of other,hydrocarbons in solution produced polymers with proper experimentation,and documentation.,2.0 PRINCIPLE OF METHOD,2.1 A weighed sample of polymer is dissolved in chloroform and,the cement is coagulated with an isopropyl alcohol solution containing,a specific amount of alpha-methyl styrene (AMS) as the internal,standard. The extract of this coagulation is then injected into a gas,chromatograph and separated into individual components. quantification,is achieved by the method of internal standardization.,3.0 DEFINITIONS,3.1 The definitions are included in the text as needed.,4.0 INTERFERENCES,(Reserved),5.0 SAFETY,5.1 This method may involve hazardous materials, operations, and,equipment. This method does not purport to address all of the safety,problems associated with its use. It is the responsibility of the user,of this method to establish appropriate safety and health practices,and determine the applicability of regulatory limitations prior to,use.,6.0 EQUIPMENT AND SUPPLIES,6.1 Analytical balance, 160 g capacity, 0.1 mg resolution,2,6.2 Bottles, 2-oz capacity with poly-cap screw lids,6.3 Mechanical shaker,6.4 Syringe, 10-ul capacity,6.5 Syringe, 2.5-ml capacity, with 22 gauge 1.25 inch needle,PP/PE material, disposable,6.6 Gas chromatograph, Hewlett Packard model 5890, or,equivalent, configured with FID, split injector packed with silanized,glass wool.,6.6.1 Establish the following gas chromatographic conditions, and,allow the system to thoroughly equilibrate before use.,6.6.2 Injector parameters:,Injection technique = Split,Injector split flow = 86 ml/min,Injector temperature = 225 deg C,6.6.3 Oven temperature program:,Initial temperature = 40 deg C,Initial time = 6 min,Program rate = 10 deg C/min,Upper limit temperature = 175 deg C,Upper limit interval = 10 min,6.6.4 Detector parameters:,Detector temperature = 300 deg C,Hydrogen flow = 30 ml/min,Air flow = 350 ml/min,Nitrogen make up = 26 ml/min,6.7 Gas chromatographic columns: SE-54 (5%-phenyl) (1%-vinyl)-,methylpolysiloxane, 15 M X 0.53 mm ID with a 1.2 micron film,thickness, and a Carbowax 20M (polyethylene glycol), 15 M X 0.53 mm ID,with a 1.2 micron film thickness.,6.7.1 Column assembly: using a 0.53 mm ID butt connector union,join the 15 M x 0.53 mm SE-54 column to the 15 M x 0.53 mm Carbowax,20M. The SE-54 column will be inserted into the injector and the,Carbowax 20M inserted into the detector after they have been joined.,6.7.2 Column parameters:,Helium flow = 2.8 ml/min,Helium headpressure = 2 psig,3,6.8 Centrifuge,6.9 Data collection system, Hewlett Packard Model 3396, or,equivalent,6.10 Pipet, 25-ml capacity, automatic dispensing, and 2 liter,reservoir,6.11 Pipet, 2-ml capacity, volumetric delivery, class A,6.12 Flasks, 100 and 1000-ml capacity, volumetric, class A,6.13 Vial, serum, 50-ml capacity, red rubber septa and crimp ring,seals,6.14 Sample collection basket fabricated out of wire mesh to,allow for drainage,7.0 CHEMICALS AND REAGENTS,CHEMICALS:,7.1 alpha-Methyl Styrene, C9H10, 99+% purity, CAS 98-83-9,7.2 n-Hexane, C6H14, 99+% purity, CAS 110-54-3,7.3 Isopropyl alcohol, C3H8O 99.5+% purity, reagent grade, CAS,67-63-0,7.4 Chloroform, CHCl3, 99% min., CAS 67-66-3,REAGENTS:,7.5 Internal Standard Stock Solution: 10 mg/25 ml AMS in,isopropyl alcohol.,7.5.1 Into a 25-ml beaker, weigh 0.4 g of AMS to the nearest 0.1,mg.,7.5.2 Quantitatively transfer this AMS into a 1-L volumetric,flask. Dilute to the mark with isopropyl alcohol.,7.5.3 Transfer this solution to the automatic dispensing pipet,reservoir. This will be labeled the AMS STOCK SOLUTION.,4,7.6 n-Hexane Stock Solution: 13mg/2ml hexane in isopropyl,alcohol.,7.6.1 Into a 100-ml volumetric flask, weigh 0.65 g of n-hexane,to the nearest 0.1 mg.,7.6.2 Dilute to the mark with isopropyl alcohol. This solution,will be labeled the n-HEXANE STOCK SOLUTION.,8.0 SAMPLE COLLECTION, PRESERVATION AND STORAGE.,8.1 A sampling device similar to Figure 1 is used to collect a,non-vented crumb rubber sample at a location that is after the,stripping operation but before the sample is exposed to the,atmosphere.,8.2 The crumb rubber is allowed to cool before opening the,sampling device and removing the sample.,8.3 The sampling device is opened and the crumb rubber sample,is collected in the sampling basket.,8.4 ……
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