Hostname: page-component-586b7cd67f-rcrh6 Total loading time: 0 Render date: 2024-11-25T15:53:16.737Z Has data issue: false hasContentIssue false

Fundamental Relationships in Acid Decomposition of Samples for Elemental Analysis using Microwave Energy

Published online by Cambridge University Press:  21 February 2011

H. M. Kingston
Affiliation:
Center for Analytical Chemistry, Inorganic Analytical Research Division, National Bureau of Standards
Get access

Extract

Appropriate sample preparation is essential to achieve both accuracy and precision in analysis of materials. This preliminary step is one of the most time-consuming parts of many analyses and has become the rate limiting step for such multi-element techniques as ICP, AA, GFAAS and ICPMS. Acid dissolution of biological and botanical samples can take from 4 to 48 hours using classical digestion techniques. Standard reflux methods used in EPA procedures may take from 24–96 hours. Many of these same samples require only 10 to 20 minutes with microwave digestions, dramatically reducing preparation time. Volatile elements such as selenium and phosphorus can be quantitatively retained in a sealed vessel using microwave decomposition prior to instrumental analysis (1). The technique has been tested on all the major sample types including biological, botanical, geological, alloy, and glassy samples and has demonstrated advantages for each of these sample groups. The development of microwave procedures for each of these sample types is currently an intense area of research.

Type
Research Article
Copyright
Copyright © Materials Research Society 1988

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

REFERENCES

1. Patterson, K. Y., Veillon, C., Kingston, H. M., “Microwave Digestion of Biological Samples for Selenium Analysis by Electrothermal Atomic Absorption Spectrometry” in Introduction to Microwave Sample Preparation: Theory and Practice, edited by Kingston, H. M. and Jassie, L. B., (ACS Reference Book Series, 1988) in press.Google Scholar
2. Kingston, H. M. and Jassie, L. B., Analytical Chemistry 58 (12) (1986).CrossRefGoogle Scholar
3. Minard, D., Physiological and Behavioral Temperature Regulations, edited by Hardy, J. D., Gage, A. P., Stolwijk, J. A. J., Thomas, C. C., (Springfield, IL, 1970) Chapter 25.Google Scholar
4. Guy, A. W., Lehmann, J. F., Stonebridge, J. B., Proc. IEEE 62 (1), 5575 (1974).CrossRefGoogle Scholar
5. Lehmann, J. F., Guy, A. W.,, Stonebridge, J. B., Delateur, B. J., J. IEEE Trans. Microwave Theory Tech. MTT–26 (28), 556563 (1978).CrossRefGoogle Scholar
6. Johnson, C. C. and Guy, A. W., Proc. IEEE 60 (6), 692718 (1972).CrossRefGoogle Scholar
7. Parker, V. B., Nat'l. Stand. Ref. Data Ser. (U.S. Natl. Bur. Stand.), NSRDS-NBS 2 (1965).Google Scholar
8. Kingston, H. M. and Jassie, L. B., “Monitoring and Predicting Parameters in Microwave Dissolution” in “Introduction to Microwave Samples Preparation: Theory and Practice,” edited by Kingston, H. M. and Jassie, L. B. (ACS Reference Book Series, 1988) in press.Google Scholar
9. Jackwerth, E. and Gomiscek, S., Pure Appl. Chem. 56 (4), 480489 (1984).CrossRefGoogle Scholar
10. Skoog, D. A. and West, M. W., “Fundamentals of Analytical Chemistry,” 2nd ed. (Holt, Rinehart and Winston, Inc., 1969), 756.Google Scholar
11. Bock, R., “A Handbook of Decomposition Methods in Analytical Chemistry,” (Translated and revised by Marr, I. L., John Wiley and Sons, New York, 1979) Chapter 4.Google Scholar
12. Kingston, H. M. and Jassie, L. B., J. Res. Natl. Bur. Stand. 93 (1988) in press.CrossRefGoogle Scholar