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The method of Murray and Ashley for the colorimetric determina- ducible red color, and i s particularly suitable for routine work be-
tion of nickel in steel is outlined and criticized. Experimental data cause of its rapidity and manipulative simplicity. Copper and cobalt
are presented on the stability under various conditions of the red interfere only slightly; the other elements ordinarily found in steel
color of oxidized nickel dimethylglyoxime. A modification of the d o not interfere. The accuracy of the method is comparable to that
method is described which gives a highly stable and readily repro- of routine gravimetric procedures.
Tests were made to determine the sensitivity of the method to Table I. Analysis of Steels
small variations in procedure. It was found that the tartaric Sample 50a Sample 132
Bureau of Aut,horr‘ Bureau of Authors’
acid, bromine water, and dimethylglyoxime added could be Standards method Standards method
decreased 25y0 or increased 100% without affecting the re- I “/r 70 %
sults. The ammonium hydroxide may be decreased 20% or in- Tungsten 18.25 6.29
creased 507, without effect. Approximately the same range of Chromium 3.52 4.09 ..
Vanadium 0.970 1.64
values holds for the sodium hydroxide. It was determined that Nickel 0.045 0:Oi 0.095 o:i3
Molybdenum .. .. 7.08 ..
the time elapsed between adding the dimethylglyoxime and the
sodium hydroxide i. not ciitical SO long ar it exceedq 1 minute-
Le., color development iq complete in less than 1minute.
ference of the other elements mentioned was determined by wing
Three identical samples equivalent to a standard steel contain-
ing 0.60% nickel were prepared, using for each sample 0.125 gram the method without modification of any sort to analyze for nickel
of National Bureau of Standards Bessemer steel 10d and 0.125 in two Bureau of Standards tool steel samples, 50a and 132.
gram of nickel-chromium stee1.32~. To sample 1 the sodium hy- In view of the extreme conditions in these two analyse5 and
droxide, which arrests color development as well as preventing the small error in nickel in each case, it was concluded that these
iron precipitation, was added 30 seconds after adding di-
methylglyoxime; to sample 2,jminutesafter adding the dimethyl- elements do not interfere 11-ith the determination to any appre-
glyoxime; and to sample 3, 10 minutes after adding the di- ciable extent. In the analysis of ordinary chromium-nickel stain-
methylglyoxime. In each case the solution was diluted to the le?. steel., no interference by chromium was observed.
volumetric mark and mixed immediately after adding the sodium
hydroxide. Transmittance readings in each case were taken 10
A D V A N T A G E S OF M E T H O D
minutes after adding the sodium hydroxide. The results, ex-
pressed in terms of the analysis of the steel as read from the 0 to The most important advantages of the method are its rapidity
l.y0nickel curve, averaged 0.599% nickel with a maximum devia- and its freedom from manipulation9 requiring exceptional pre-
tion from the average value of 0.0057, nickel.
rautions or a high degree of analytical skill. It is well suited for
INTERFERENCES routine use. When a group of five samples was analyzed by a
worker only recently familiar with the method, the total elapsed
The method wab tested for interference by copper, cobalt, tung- time, exclusive of weighing, was 1 hour and 10 minutes (reTults
sten, molybdenum, chromium, and vanadium. The small reported above in paragraph on reproducibility). If a large num-
amounts of copper (less than 0.2%) present in the usual steels did ber of samples is run a t one time, one thoroughly familiar cvith
not interfere. Copper, when present to the extent of 0.50(7, in the method can reduce the time required per sample to about 8
the steel, caused a positive nickel error of 0.027,. Cobalt, tvhen minutes.
added to thr sample equivalent to 2.57, in the steel, caused a posi-
tive error of 0.037, nickel. Both elements were tested for inter- LITERATURE CITED
ference on a <ample of +el containing 0.6Ovp nickel. The inter- (1) Murray and Ashley, IXD.ESG.CHEM..
~ A L ED.,
. 10,1 (1938).