The Practical Analysis of High-Purity Chemicals. VI. Emission Spectrographic Analysis of High-Purity Acids

Abstract

The spectrographic analysis of volatile acids in a high-purity form is reviewed and a procedure presented that involves evaporation of a 100-g sample under temperature controlled contamination-free conditions and emission spectrography using dc-arc excitation under controlled atmosphere. In the evaporation, graphite (10 mg) is added as a collector, sulfuric acid to convert to less volatile sulfates (with acetic, hydrochloric, and nitric acids), and also mannitol to retain boron (with hydrochloric and hydrofluoric acids). Indium is added as a internal standard. Spectra are examined for 33 elements against a multielement standard in graphite containing indium as an internal standard. For the concurrent analysis of three samples, the elapsed time is 4–10 h and the actual working time 3–5 h. Recovery studies are reported as well as the use of the procedure in the assessment of the leaching of borosilicate glass by concentrated mineral acids.

Keywords

Acetic acid Acids high-purity Analysis of acids Contamination Emission spectroscopy Glass Hydrochloric acid Hydrofluoric acid Mineral acids Nitric acid Perchloric acid Review paper Standards spectroscopic Sulfuric acid

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References

Barnard

A. J.

Jr. Joy

E. F.

Little

, and Brooks

J. D.

, Talanta 17, 785 (1970).

Barnard

A. J.

Jr. , and Joy

E. F.

, Chemist 47, 243 (1970).

Joy

E. F.

Bonn

J. D.

, and Barnard

A. J.

Jr. , Thermochim. Acta 2, 57 (1971).

Barnard

A. J.

Jr. Joy

E. F.

, and Michelotti

F. W.

, Clin. Chem., in press.

Barnard

A. J.

Jr. , “High-Purity Chemicals—A Challenge to Practical Analysis,” in Methods and Techniques of Ultra-Purity, edited by Zief

and Speights

R. M.

(Dekker, New York, 1971), in press.

Joy

E. F.

and Barnard

A. J.

Jr. , “Commercial Acids and Bases,” in Standard Methods of Chemical Analysis, edited by Welcher

F. J.

, (Nan Nostrand, Princeton, N. J., 1963), 6th ed., Vol. II, Chap. 22, pp. 534–626.

Joy

E. F.

and Barnard

A. J.

Jr. , in Encyclopedia of Industrial Analysis (Wiley-Interscience, New York); “Acetic Acid” and “Acetic Anhydride,” Vol. 4, pp. 93–107; “Chlorosulfonic Acid,” Vol. 9, pp. 528–534; “Fluoro Acids, Inorganic,” Vol. 13, in press; “Inorganic Acids,” in preparation.

Speights

R. M.

and Barnard

A. J.

Jr. , in Encyclopedia of Industrial Analysis (Wiley-Interscience, New York); “Citric Acid and its Salts and Esters,” Vol. 10, pp. 85–110; and “Formic Acid and its Salts and Esters,” in press.

Kershner

N. A.

and Joy

E. F.

, procedure in Ref. 6, p. 552.

10.

Oldfield

J. H.

and Bridge

E. P.

, Analyst 85, 97 (1960).

11.

Mareček

and Ditz

, Chem. Listy 59, 972 (1965).

12.

Petsov

G. A.

Manova

T. G.

, and Krasil'shchik

V. Z.

, in Analysis of High-Purity Materials, edited by Alimarin

I. P.

(Israel Program for Scientific Translations, Jerusalem, 1968), pp. 577–580; Petsov

V. Z.

and Krasil'shchik

V. Z.

, Zh. Analit. Khim. 18, 1314 (1963).

13.

Thiers

R. E.

, “Separation, Concentration, and Contamination,” in Trace Analysis edited by Yoe

J. H.

and Koch

H. J.

Jr. (Wiley, New York, 1957), pp. 637–666.

14.

Thiers

R. E.

, “Contamination in Trace Element Analysis and Control,” in Methods of Biochemical Analysis, edited by Glick

(Wiley-Interscience, New York, 1967), Vol. 5, pp. 273–335.

15.

Vasilevskaya

L. S.

Kondrashina

A. I.

, and Muravenko

V. P.

, Ref. 12, pp. 573–575; Vasilevskaya

L. S.

Muravenko

V. P.

, and Kondrashina

A. I.

, Zh. Analit. Khim. 20, 540 (1965).

16.

Notkina

M. A.

Solodovnik

S. M.

Vasilevskaya

L. S.

, and Nazarova

N. G.

, Ref. 12, pp. 575–577; Notkina

M. A.

and Solodovnik

S. M.

, Zavod. Lab. 28, 176 (1962).

17.

Chaney

C. L.

and Peterson

M. J.

, U. S. Dept. Interior, Bur. Mines, RI 6249 (Washington, D. C, 1963), 18 pages.

18.

and Hall

, Owens-Illinois Technical Center, unpublished work.

19.

Merck and Co. , Rahway, N. J., unpublished procedures.

20.

Feldman

, Anal. Chem. 33, 1916 (1961).

21.

Vasilevskaya

L. S.

Kondrashina

A. J.

, and Shifrina

G. G.

, Zavod. Lab. 28, 674 (1962).

22.

Gallus-Olender

, Chem. Anal. (Warsaw) 10, 1039 (1965).

23.

Fred

Nachtrieb

N. H.

, and Tomkins

F. S.

, J. Opt. Soc. Amer. 37, 279 (1947); Nachtrieb

N. H.

, Principles and Practice of Spectrochemical Analysis (McGraw-Hill, New York, 1950), Chap. 13.

24.

Coppola

P. P.

and Hughes

R. C.

, Anal. Chem. 24, 768 (1952); Kwestroo

and Visser

, Analyst 90, 297 (1965).

25.

Kuz'min

N. M.

Zhuravlev

G. I.

Kuzovlev

I. A.

Galaktionova

A. N.

, and Zakharova

T. I.

, Zh. Analit. Khim. 24, 429 (1969).

26.

Wolfram

W. E.

and Barnard

A. J.

Jr. , J. T. Baker Chemical Co., unpublished work.

27.

Raggon

F. C.

and Bacon

F. R.

, Amer. Ceram. Soc. Bull. 33, 267 (1954); Bacon

F. R.

, Glass Ind. 49, 438–442 (1968).

28.

McIlroy

R. E.

, U. S. Design Patent 216,362 (23 December 1969), assigned to J. T. Baker Chemical Co.