X-Ray Spectroscopy as a Control Method in the Production of Zirconium and Hafnium

D. M. Mortimore; P. A. Romans

doi:10.1364/JOSA.42.000673

Journal of the Optical Society of America
Vol. 42,
Issue 9,
pp. 673-677
(1952)
•https://doi.org/10.1364/JOSA.42.000673

X-Ray Spectroscopy as a Control Method in the Production of Zirconium and Hafnium

D. M. Mortimore and P. A. Romans

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D. M. Mortimore and P. A. Romans, "X-Ray Spectroscopy as a Control Method in the Production of Zirconium and Hafnium," J. Opt. Soc. Am. 42, 673-677 (1952)

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Abstract

An x-ray spectrographic method has been developed for routine analysis of mixtures of zirconium and hafnium oxides in the range of concentrations from 0.5 to 99.5 percent hafnium in zirconium. The method makes use of the newly perfected x-ray fluorescence analysis equipment incorporating a Geiger tube together with associated scaling and recording circuits for measurment of intensities. A single analysis requires 5 to 10 minutes to complete, including preparation of sample and final calculations. The average percent deviation at concentrations of 1 percent hafnium is 3.3 percent and at 40 percent hafnium about 0.5 percent.

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Corrections

D. M. Mortimore and P. A. Romans, "Errata," J. Opt. Soc. Am. 42, 989_5-989 (1952)
https://opg.optica.org/josa/abstract.cfm?uri=josa-42-12-989_5

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Sample number	Observed values	Mean	Deviation from mean	Percent deviation	Average percent deviation	Standard deviation
	0.92		0.045	4.66
	1.08		0.043	4.46
	0.92		0.045	4.66
	0.98		0.015	1.55
S-923^a	0.98	0.965	0.015	1.55	3.32	3.82
	0.93		0.035	3.63
	0.92		0.045	4.66
	0.93		0.035	3.63
	0.97		0.005	0.52
	1.02		0.037	3.83
	39.8		0.14	0.35
	39.7		0.04	0.10
	39.8		0.14	0.35
	39.3		0.36	0.91
7964^a	40.2	39.66	0.54	1.36	0.55	0.73
	39.5		0.16	0.40
	39.9		0.24	0.61
	39.6		0.06	0.15
	39.6		0.06	0.15
	39.2		0.46	1.16
	3.88		0.00	0.00
	3.98		0.10	2.58
	3.88		0.00	0.00
	3.82		0.06	1.55
SA-2888^b	3.78	3.88	0.10	2.58	1.65	2.12
	3.80		0.08	2.06
	3.88		0.00	0.00
	3.98		0.10	2.58
	4.00		0.12	3.09
	3.80		0.08	2.06

Weight of sample mixed with 1 gram of corn starch, gram	Sample 7864^a	Observed values Sample 11541^a	Sample lot 4^b
1	38.8	37.2	3.82
0.7	38.6	37.2	3.82
0.5	38.4	35.5	3.86
0.1	34.9	32.2	4.55
0.05	34.6	29.5	4.50

Impurity element added	Observed values (Hf/Hf+Zr)×100
Impurity element added	Pure (Hf+Zr)O₂	1% added	5% added	10% added	40% added
Nickel	39.3	39.0	38.1	36.4	29.8
Iron	39.3	39.0	39.0	37.6	31.3
Tin	39.3	39.2	38.4	38.2	34.2
Titanium	39.3	39.3	38.3	37.8	34.7
Strontium	39.3	39.3	40.1	41.7	46.2
Rubidium	39.3	39.0	41.2	44.2	48.2

Sample number	Observed values	Mean	Deviation from mean	Percent deviation	Average percent deviation	Standard deviation
	0.92		0.045	4.66
	1.08		0.043	4.46
	0.92		0.045	4.66
	0.98		0.015	1.55
S-923^a	0.98	0.965	0.015	1.55	3.32	3.82
	0.93		0.035	3.63
	0.92		0.045	4.66
	0.93		0.035	3.63
	0.97		0.005	0.52
	1.02		0.037	3.83
	39.8		0.14	0.35
	39.7		0.04	0.10
	39.8		0.14	0.35
	39.3		0.36	0.91
7964^a	40.2	39.66	0.54	1.36	0.55	0.73
	39.5		0.16	0.40
	39.9		0.24	0.61
	39.6		0.06	0.15
	39.6		0.06	0.15
	39.2		0.46	1.16
	3.88		0.00	0.00
	3.98		0.10	2.58
	3.88		0.00	0.00
	3.82		0.06	1.55
SA-2888^b	3.78	3.88	0.10	2.58	1.65	2.12
	3.80		0.08	2.06
	3.88		0.00	0.00
	3.98		0.10	2.58
	4.00		0.12	3.09
	3.80		0.08	2.06

Weight of sample mixed with 1 gram of corn starch, gram	Sample 7864^a	Observed values Sample 11541^a	Sample lot 4^b
1	38.8	37.2	3.82
0.7	38.6	37.2	3.82
0.5	38.4	35.5	3.86
0.1	34.9	32.2	4.55
0.05	34.6	29.5	4.50

Abstract

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Journal of the Optical Society of America