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STEREO-PYROMETER

(English Patent 10617/1905). For ascertaining any temperature from 550° C. to 2000°.
Works like a limit gauge, pass or reject. Costs little to buy.
Gives the Hardener a Confidence that is founded on fact.
Makes the Hardening Shop as precise as the Tool Rɔom.

No Delicate Mechanism to get out of Order.
Used like a Stereoscope (for Direct Observation only).

This is undoubtedly the simplest and most reliable form of Pyrometer for practical use in works. It can be used for ascertaining the temperature of :

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IT has been shown by Newton (Am. Journ. Sci., 1908, xxv., 343) that ferric iron in sulphate solution can be quickly and accurately estimated by reducing with titanous sulphate, oxidising the excess of titanous salt with bismuth trioxide, filtering off the excess of bismuth trioxide and reduced bismuth, and titrating the resulting clear solution with a o'1/N solution of potassium perman ganate. As it was afterwards discovered that uranyl salts in sulphate solution were apparently reduced by titanous sulphate to the uranous condition, the present investigation was undertaken for the purpose of applying the above method to the estimation of uranium and to the estimation of phosphorus after the latter had been precipitated as ammonium-uranyl phosphate.

For this work a solution of titanous sulphate of convenient strength was prepared as follows:-To 100 cc. of sulphuric acid were added little by little and with continual stirring 25 grm. portions of the best hydrous C.P. titanium oxide, the whole being kept constantly heated to the fuming-point of the acid. The resulting pasty mass was allowed to come to room temperature and cautiously transferred to a beaker containing about 200 cc. of cold water. After standing a short time the somewhat cloudy solution of titanic sulphate was filtered, reduced to the titanous condition by means of zinc, and then filtered directly into about two litres of recently boiled distilled water, contained in a reservoir to which a Squibb's automatic burette and a hydrogen generator were immediately attached. By this means the easily oxidised titanous sulphate was kept under a constant pressure of hydrogen, and measured amounts of the solution were drawn as wanted. As it was convenient to know the strength of the titanous sulphate solution it was titrated directly against a o'1/N solution of potassium permanganate. An approximately o'1/N solution of uranyl sulphate was obtained by treating an equivalent amount of uranyl acetate of tested purity with sulphuric acid, filtering, and diluting to the required volume. This solution was standardised in the gravimetric way by precipitating the uranium by ammonia, washing with dilute ammonium nitrate solution, igniting, and weighing as U303.

A phosphate solution was obtained by dissolving about 6.359 grms. of microcosmic salt in a litre of water, the solution being afterwards standardised by use of the magnesium pyrophosphate method as outlined by B. Schmitz (F. P. Treadwell's "Analytische Chemie," 1911). The potassium permanganate solution of approximately 01/N value was exactly standardised by titrating against carefully weighed portions of purified sodium oxalate previously dissolved in a convenient volume of water, acidu lated with I: I sulphuric acid, and heated to 80°. This method is the one recommended by the Bureau of Standards when using sodium oxalate as a standard in volumetric analysis, and is exactly described in their Circular, No. 40. The sodium oxalate here used was kindly

furnished by the above-mentioned Bureau.

A bismuth trioxide must be taken which shows no appreciable reducing action toward potassium permanganate. A number of 2 grm. lots of the sample used, when dissolved in sulphuric acid, cooled, and diluted, were permanently coloured by the first drop of a o'1/N solution of potassium permanganate.

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In Table II. are recorded results obtained when titanous sulphate was used as the reducing agent. For these ex periments measured amounts of uranyl sulphate were run into an Erlenmeyer flask of 150 cc. capacity and followed by a slight excess of titanous sulphate solution. Enough concentrated sulphuric acid was then added to make the solution approximately 16 per cent acid by volume. (It was found that uranyl salts are more easily reduced and when reduced much more stable in an acid solution of this concentration than in one that is weaker). The flask and contents were then cooled under the tap, a small amount of bismuth trioxide was added (enough in each case to oxidise the excess of titanous sulphate), and the flask then left to stand a minute or two, with occasional shaking. By the use of the filter pump and a platinum cone well padded with asbestos the solution was quickly filtered free from bismuth trioxide and reduced bismuth, the asbestos pad carefully washed three or four times with a 16 per cent sulphuric acid solution, and the combined filtrates titrated with standard potassium permanganate. As the titanous sulphate solution contained a small amount of iron a slight correction had to be made in the permanganate reading. This correction was easily and accurately made by a method of estimating iron in the presence of titanium, as worked out by Gooch and Newton (Am. Journ. Sci., 1907, xxiii., 365).

TABLE II. Data on Titration of Uranium After Reduction by Titanous Sulphate in Presence of Bismuth Trioxide. KMnO4 used. UO2 present. UO2 found

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Grm. 0 0545

Grm

+0'0004

0'0549

+0.0008

O'1092

+0'0009

0.1088

0'1079 0.1631 0.1626 0.1626 0'1626 0'2173 0.2169 0.2173

0'2173

+0'0005 -0'0004 +0'0007 +0'0002 +0'0002 +0'0002 +0'0007 +0'0003 +0'0007 +0'0007

I cc. of o1/N permanganate corresponds to 001350+grm. of uranium dioxide and one drop or onethirtieth of a cc. corresponds to 0.00045+grm. of uranium is probably due to the reading of the end-point. dioxide, it appears that any appreciable error in the process

The Estimation of Phosphorus.

It has long been known that under proper conditions an alkali phosphate is completely precipitated by adding to it an excess of uranyl nitrate. In using the above reaction for the estimation of phosphorus when a separation of the

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