FORD FLTM AO 107-01-2001 QUANTITATIVE ANALYSIS OF TRIMETHYLAMINE《三甲胺的定量分析》.pdf

1、 FORD LABORATORY TEST METHOD AO 107-01 Date Action Revisions 2001 01 30 Revised Editorial no technical change A. Cockman 2000 04 17 Editorial no technical change A. Cockman 1993 05 18 Printed copies are uncontrolled Page 1 of 5 Copyright 2001, Ford Global Technologies, Inc. QUANTITATIVE ANALYSIS OF

2、TRIMETHYLAMINE Application This test method is used to determine the amount of trimethylamine found in fiberglass. Apparatus Required Glass Jar 1 liter glass with ring cap. Sink Matting Plastic Nalgene Bottles 125 mL Volumetric Flasks 50 mL 100 mL Pipets Volumetric as required. Oven Forced Air. Anal

3、ytical Balance Gas Chromatograph Split/Splitless injector and nitrogen/phosphorus or flame ionization detector. CG Column Supelcowax 10, 30 m or equivalent column for the analysis of aqueous amine samples. Vials, Septum-Sealed FORD LABORATORY TEST METHOD AO 107-01 Page 2 of 5 Copyright 2001, Ford Gl

4、obal Technologies, Inc. Materials Required Sodium Hydroxide 2 M aqueous solution. Trimethylamine Hydrochloride Water Distilled deionized, freshly boiled. Polyethylene Film Conditioning and Test Conditions All test values indicated herein are based on material conditioned in a controlled atmosphere o

5、f 23 +/- 2 C and 50 +/- 5 % relative humidity for not less than 24 h prior to testing and tested under the same conditions unless otherwise specified. Procedure I. Preparation of Trimethylamine (TMA) Stock Solution and Standards 1. Accurately weigh 0.1617 g trimethylamine hydrochloride into a 100 mL

6、 volumetric flask and dilute to volume with freshly boiled distilled, deionized water to give a 1000 ppm TMA stock solution. 2. Pipet stock solution into 50 mL volumetric flasks as described below: mL of Stock ppm TMA standard 5.0 100 2.0 40 1.0 20 0.5 (500 microliter) 10 0.2 (200 microliter) 4 0.05

7、 (50 microliter) 1 3. Dilute to volume with freshly boiled distilled, deionized water. 4. Prepare working standards by pipeting 1.71 mL of each standard solution into septum-sealed vials. Add 90 microliter of 2 M sodium hydroxide to each and mix. FORD LABORATORY TEST METHOD AO 107-01 Page 3 of 5 Cop

8、yright 2001, Ford Global Technologies, Inc. II. Sample Preparation 1. Cut samples into 25 millimetre cubes and mix thoroughly. 2. Pipet 10.0 mL boiled distilled water into a glass liter jar. 3. Place a 6.5 cm tall sample support (open-ended 125 mL nalgene bottle with end cut off) in the jar, and bal

9、ance an 8.9 cm diameter disk of sink matting upon the sample support. 4. Place 10 +/- 0.05 g of sample on the sink matting, cover the jars with polyethylene film, and screw the lids on securely. 5. Place the jars in an oven at 65 C for 16 h. 6. Remove the jars from the oven and allow to cool to 23 +

10、/- 2 C for 30 minutes. 7. Transfer 1.71 mL of test water from the jar to a septum-sealed vial. 8. Add 90 microliter of 2 M NaOH to the vial. III. Gas Chromatographic Analysis of Standards and Samples 1. Gas chromatographic conditions are as follows: Column: Supelcowax-10, 30 m or equivalent 40 C for

11、 3 min, then to 150 C 10 C/min Injector: Split/Splitless 10:1 split ratio minimum 220 C Detector: Phosphorus-Nitrogen or Flame Ionization (See Note 1) 220 C Injection: 1 microliter FORD LABORATORY TEST METHOD AO 107-01 Page 4 of 5 Copyright 2001, Ford Global Technologies, Inc. 2. A linear calibratio

12、n curve is prepared by analyzing the working standards. The TMA elutes at approximately 3.5 minutes. Peak area vs. concentration is fitted to a linear calibration curve. 3. The samples are analyzed in the same manner. The TMA content is determined using the established calibration curve. Results are

13、 reported as parts per million TMA in fiberglass. Chemicals, materials, parts, and equipment referenced in this document must be used and handled properly. Each party is responsible for determining proper use and handling in its facilities. FORD LABORATORY TEST METHOD AO 107-01 Page 5 of 5 Copyright 2001, Ford Global Technologies, Inc. QUANTITATIVE ANALYSIS OF TRIMETHYLAMINE Trimethylamine Test Set-up