DIETHYLENETRIAMINE, ETHYLENEDIAMINE, & TRIETHYLENETETRAMINE: METHOD 2540, Issue 2, dated 15 August 1994 - Page 2 of 4
REAGENTS: 1. 2.
EQUIPMENT:
XAD-2 resin, reagent grade 1-Naphthylisothiocyanate (NTIC), reagent grade. Methylene chloride, reagent grade. Dimethylformamide (DMF), HPLC grade. Isooctane, HPLC grade. Isopropanol, HPLC grade. Ethylenediamine (EDA),* high purity. Diethylenediamine (DETA),* high purity. Triethylenetetramine (TETA),* high purity. Calibration stock solution, 4.8 mg/mL DETA,4.50 mg/mL EDA, 4.9 mg/mL TETA. Dissolve 95.4 mg DETA, 90.0 mg EDA, and 98.2 mg TETA in 600 mg of NTIC, allow to react for at least 60 minutes, and dilute to 20 mL with DMF.
3. 4. 5. 6. 7. 8. 9. 10.
1.
2. 3.
4. 5. 6. 7. 8.
Glass tube, 7 cm long, 6-mm OD, 4-mm ID, flame sealed ends with plastic caps, containing 2 sections of 16/50 mesh XAD-2 resin coated with 10% 1-naphthylisocyanate (front = 80 mg; back = 40 mg) separated by a plug of PTFE wool (see APPENDIX). Personal sampling pump calibrated to 0.01 to 0.1 L/min. High performance liquid chromatograph (HPLC), UV, 254 nm, cyano column and integrator (page 2540-1). Vials, 4-mL. Syringes, microliter, readable to 0.1 µL. Pipets, 2-mL. Flasks, volumetric, 25- and 50-mL. Ultrasonic water bath.
See SPECIAL PRECAUTIONS.
SPECIAL PRECAUTIONS: The vapors of these amines are painful and irritating to the eyes, nose, throat, and respiratory system. The liquids can cause severe damage to the eye and serious burns to the skin [1,5].
SAMPLING: 1. 2. 3. 4. 5.
Calibrate each personal sampling pump with a representative sampler in line. Break the ends of the sampler immediately before sampling. Attach the sampler to personal sampling pump with flexible tubing. Sample at an accurately known flow rate between 0.01 to 0.1 L/min for a total sample size of 1 to 20 L. Cap the samplers and pack securely for shipment.
SAMPLE PREPARATION: 6. 7. 8.
Transfer each sorbent section to separate 4-mL sampling vials. Add 2.0 mL DMF to each vial. Agitate in an ultrasonic water bath for 30 minutes.
CALIBRATION AND QUALITY CONTROL: 9.
10.
Calibrate daily with at least five working standards in the range of the samples. a. Prepare working standards by serial dilution of the stock standards with DMF. b. Analyze together with samples, blanks, and QC samples (steps 12 and 13). c. Prepare separate calibration graph (peak area vs. µg per sample) for EDA, DETA, and TETA. Determine the desorption efficiency (DE) at least once for each lot of XAD-2 resin used for sampling. Prepare three tubes at each of five levels plus 3 media blanks. a. Inject a known amount of analyte onto the NTIC-coated resin. b. Allow to stand overnight. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94
