Fluoride Analysis Improves - C&EN Global Enterprise (ACS

Nov 6, 2010 - SMALL AMOUNTS OF FLUORIDE in a process can cause serious corrosion problems. For example, uranium sulfate, a boiling-water-reactor ...
0 downloads 0 Views 122KB Size
Amazingly

different

SPRAY

. .

PRODUCTION

.

GUN

Fluoride Analysis Improves

Requires NO Cords, Hoses or Compressors!

OMAJLL

CO2 Cartridge Provides 100O lb. Initial Pressure

WORKS LIKE MAGIC! USE IT ANYWHERE! Sprays almost any light liquid . . . nozzle adjusts from stream to mist. Powerful CO; cartridge provides 1000 lb. initial pressure. One cartridge sufficient for spraying up to full 21 oz. containerful. Lightweight cast aluminum head, heavy gauge steel tank, brass and stainless inserts. At your Distributors, or order direct. 10 Day Money Back GuaranteeExtra CO2 cartridges available locally, or package of 10 for SI .25 postpaid.

SULLIVAN-BECKER CO. Depi. 637-K, Kenosha, Wis.

STOP THIS Plastic coated steel nipple in salt water disposal well. Failed after six months.

4

GET THIS t

L

Fïfoercasi LINE P I P E - W E L L T U B I N G

w / J / not

corrode!

Corrosion is no problem when you use Fibercast, regardless of the application. There are many other desired advantages, among them: High operating pressures (1000 p.s.i.) . . . high operating temperatures (exceed 250°F) and light w e i g h t . . . (less than V-a weight of steel). Fibercast is long-term pipe economy. Write for full details.

THE~ilBERCAST

CORPORATION

P. O. Box 727, Dept. 110 Sand Springs, Oklahoma A Subsidiary of The Youngstown Sheet and Tube Company

64

C&EN

OCT. 7,

1957

AAiOUrTTS

OF

FLUORIDE

i n SL

process can cause serious corrosion problems. For example, uranium sulfate, a boiling-water-reactor fuel, is made via uranyl fluoride, a n d some fluoride ion usually remains in the p r o d uct. Result: Even stainless steel corrodes. Key to preventing this corrosion is close control of fluoride concentration. But this requires good detection m e t h ods, and existing ones are not very satisfactory. Researchers have followed three paths toward improving methods of analysis:

with TO cartridges

Fibercast tubing on same string. Not corroded . . . no loss in strength.

Chemists still s e a r c h f o r b e t t e r analytical methods f o r t r a c e amounts o f f l u o r i d e

• Quicker, more sensitive separation. • Titration indicator which is m o r e stable against interfering ions. • More rapid a n d sensitive a m p e r o metric titration. R. H . Powell a n d Oscar Menis. Oak Ridge National Laboratory, have a revised pyrolytic separation using a gas such as oxygen, rather than steam, to purge the system during pyrolysis. T h u s the sample is not diluted w i t h large quantities of condensate. Powell and Menis told the ACS Division of Analytical Chemistry in N e w York that they get higher sensitivity as a result. Also they do not need to process t h e sample solution, thus saving time. • Pyrolyze Sample. Powell a n d Menis pyrolyze t h e sample with uranium oxide, manganese oxide, or t u n g sten oxide at 1000° C. T h e y pass a stream of oxygen, with trace amounts of water in it, over the mixture and collect the products as a water solution. W a t e r in the oxygen stream speeds recovery. After separation, fluoride is determined b y spectrophotometric titration. They say the method can separate as little as 10 micrograms of fluoride. Most spectrophotometric methods for trace fluorides, however, are not in themselves completely satisfactory. L . Silverman a n d M. E. Shideler, Atomics International, say they are not specific enough and most ions must b e removed prior to analysis. Silverman a n d Shideler increase the titration's sensitivity by using beryllium-Chrome Azurol S colored complex as an indicator.

There are other ways of cutting interference caused by foreign ions. An amperometrie method used by W . E . Harris, University of Alberta, does this to some extent. Harris uses a rotating palladium electrode, with standard thorium solution as titrating reagent a n d ferric iron as the indicator. He titrates in a buffered solution containing potassium bromide and sulfate. Best results are obtained with 100 to 200 micrograms of fluoride per 100 ml. of solution, b u t 20 micrograms in 100 ml. can b e determined, α

>

COMMENT

It is likely that radioisotopes and radiant energy techniques will be widely applied in chemical engi­ neering research, development, and pilot plant investigations. They should prove of tremendous value in clarifying true mechanisms and characteristics of chemical engi­ neering operations. Most of our so-called chemical engineering theory still consists of highly du­ bious extrapolations of dilute physi­ cal chemistry to concentrated com­ mercial systems. In adding radiation to the three classical control elements of chemi­ cal reactions—heat, pressure, and catalysis—tve have a valuable tool for greatly extending the flexibility and utility of processes. Again, we sorely need fundamental data and not prognostications to block out the real potential of these nuclear energy applications. A great deal of information on processing uranium and thorium ores to purified salts or metal should be directly applicable to other industrial problems. Ex­ amples are: ion exchange resins and processes; extractive solvents and processes; materials handling; solids-gas contacting; flocculents; continuous reduction of metal bol­ ides to metal; corrosion and ero­ sion resistant materials; leaching techniques; use of corrosive and toxic gases such as HF, Cl2> and F2; continuous decomposition of compounds; improved methods for absorption of gases, such as nitro­ gen oxides; and many others. RAYMOND E. VENER, of Cata­ lytic Construction, addressing the meeting of the Synthetic Organic Chemical Manufacturers Associa­ tion, Sept. 10, 1957.