A Modified Thiele Melting-Point Apparatus - Analytical Chemistry (ACS

Ernest Conte. Ind. Eng. Chem. Anal. Ed. , 1930, 2 (2), pp 200–200. DOI: 10.1021/ac50070a032. Publication Date: April 1930. ACS Legacy Archive. Cite th...
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A-l-ALYTZCAL E D I T I O S

200

Vol. 2. s o . 2

A Modified Thiele Melting-Point Apparatus' Ernest Conte THE~ I A L L I S C K R O D T

C H E M I C A L ~ ~ O R K JERSEY S , C I T Y LABORATORY,

223 TO 243 W E S T S I D E A V E . , JERSEY C I T Y ,

N.J.

containing the material under test. in respect to the rner('ury bulb of the thermometer very critical. K i t h the modificcl tube the temperature variation throughout the tube is greatly reduced, thereby accomplishing tlie much desired need r ~ f:I uniform temperature bath which is so essential to c11;t:iiii dependable melting points. This laboratory lias satisfact,orily used the tLlIJ(' I'(1r boiling-point determin is, where a uniforni tint11 is also desirablc. It lias heen used for dissol1-inp ninterinl; which require considerable slialiing and arc nut affectd hy tlie introduction of air: for extraction operations, a i d for aerating liquid materials. Other applications 1nay i i i time suggest theniselves.

Device for Fastening MeltingPoint Tubes to Thermometers' H. L. Lochte

tube is held in place either by adhesion or by tying it t o the thermometer with some suitable material depending on the bath medium used. The bent tube, A-, is connected with a water p u m p ( a s p i r a t o r ) and air is drau-n through the apparatus a t

A-

U N I V E R S I T Y O F T E X A S , AuSTIS, ' I E X .

SUMBER of schemes for prel-entA ing the aggravating tendency of melting-point tubes to slip in making meltingpoint determinations have been described and are listed in handbooks and manuals. The following simple and effective plan appears not to have been d e w i b e d before. A glass rod 3 to 5 inm. in diameter is fastened to the stem of the thermometer as indicated in the figure. Even the most vigorous stirring will not cause the tube to turn loose when in the position shown in a sulfuric acid bath. If the plan is t o be used with the Thiele melting-point apparatus the rod may be fastened by wire as shown or, preferably, be passed, along with the thermometer, through a single elongated hole in the cork. 1

T

M ' B

50 42 36

100 89 76

150 138 122

200 187 168

50

50 49.9

100 99.8 99.5

150

149 5 148.8

200 199.2 198.0

T h e above readings were taken simultaneously when the temperature a t T h a d been held within 1' C. for 5 minutes. Three standard thermometers were used; one was placed a t T , a height so that the bath just covered the mercury bulb, one a t .VI, the center, and the other a t B , the bottom of t h e tube. Stem corrections were given to all these readings. It will be noticed t h a t the temperature of the bath varies considerably a t different parts of the ordinary Thiele tube. This variation makes the position of the capillary tube, 1

Received January 24, 1930.

Received December 26, 1929.

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