Less than 1 ppb of Ni(CO)4 has been detected, under STP conditions, in the presence of a 106-fold excess of CO at 2 cm−1 resolution. Absorbance subtraction software was employed to minimize the interfering effects of the CO spectra. These results indicate that, using 20 m absorption length gas cells, Ni(CO)4 concentrations on the order of 0.01 ppb are detectable using this technique.
These calibrated mixtures were prepared, analyzed, and supplied by Precision Gas Products, Inc., 681 Mill St., P.O. Box 1171, Rahway, NJ 07065. Measurement uncertainties (x ± y) are quoted in units of the last significant figure of x.
3.
It was remarked by Dr. St. John Blakeley (private communication), International Nickel Co., Canada, that trace amounts of Fe(CO)5 and Ni(CO)4 are normally found in high pressure carbon monoxide samples, and, furthermore, these impurities can be removed by passing the sample through copper gauze traps heated to 50°C. These precautions were not employed here.
4.
GriffithsP., Appl. Spectros.29, 11 (1975).
5.
CosbyL., Union Carbide Corp., South Charlestown, WV, private communication.