I S D C S T R I S L A S D E-YGISEERISG CHEMISTRY
January 15, 1930
practical work a volume correction for the Nick is urinecessary. The excess of sodium carbonate was titrated and the percentage of total sulfur calculated in the usual manner. The results in Table I are typical for natural-gas gasoline and other light distillates. Table I SPECIFIC -------TOTAL SAMPLE GRAIITY 1 2 Per ceir: Per cent 1 0.642 0.022 0.026 2 0.65 0.038 0.041 3 0.66 0,099 0.104 4 0.675 0,091 0 094 5 0.67 0.040 0 044
SULFI.R------3 Average Per c e t i l Per cent 0.024 0.024 , . . 0 0395 ,.. 0 1015 ... 0 0925
...
0,042
To further test the accuracy of the method for the very light distillates, elementary sulfur equivalent to 0.05 per cent by weight was dissolved in sample 5 and the total sulfur was determined. The results are shown in Table 11. Table I1
SAMPLE
SPECIFIC GRAVITY
____ 1 Per Len:
TOTALSVLFUR----2 Average Per cent Per cenl 0 044 0 042 0 096 0 094
25
ral-gas gasoline, except that a heated liquid bath with leveling bulb attachment was substituted for the ice-water bath. The temperature of the heated liquid bath and the relative levels of the heated liquid and the heavy distillate are factors that have to be determined individually for each distillate. K i t h a little practice these adjustments can be readily made. T o test the accuracy of this method, elementary sulfur was dissolved in a highly refined medicinal oil and total sulfur was determined by the oxygen-bomb method and by the modified lamp method. with heated liquid bath as described. Also both methods were used for the determination of total sulfur in a crude oil. The results in Table IV were obtained. Table IV PRVDUCT Medicinal oil Medicinal oil Crude oil Crude oil
SPECIFIC--TOTAL h'XETHOD
Oxygen bomb Modified lamp Oxygeu bomb Modified lamp
GRAVITY 0.889 0,889 0.841 0,841
SULFUR-2 Av.
1
Per cent
Per cent
0,109 0.105 0.517 0,473
0.110 0,101 0.514 0,473
Per cent 0.1096
0.103 0.5155 0.4755
The results in Table I1 indicate a reasonably accurate estimation of the added elementary sulfur.
The results in Table IV indicate that the modified lamp method yields satisfactory results for heavy distillates free from tarry or asphaltic materials. The results with the crude oil were not satisfactory, as the tarry or asphaltic matter present in the crude gummed the wick and made it difficult to maintain a small steady burning flame.
Gasoline and Kerosene
General Conclusions
3
5=
0 67 0 67
0 040 0 092
0.052b
a With added sulfur. b Difference.
For ordinary gasoline and kerosene the ice-water bath was not used. Otherwise, the apparatus and manipulation were exactly the same as those used for natural-gas gasoline. h measured volume of the distillate was burned under the absorption apparatus of the standard lamp method and the weight was calculated from the knon-n density. The percentage of total sulfur was determined in the usual manner.
The results recorded in Tables I, 11, 111, and I V indicate that the modified lamp method as here described will give satisfactory results iyith natural-gas gasoline and other light distillates, with ordinary gasoline and kerosene, and with the heavier distillates free from tarry or other gummy materials. The method is not satisfactory for crudes or for the usual unrefined heavy distillates. The modified lamp method was found to be very satisfactory for natural-gas gasoline and other light distillates for which a t the present time no generally satisfactory method is in common use.
Rapid Determination of Relative Viscosities of Opaque Liquids' Milton 11. Loeserman BASS-HUETER PAINTC O Y P A Y Y ,
s.4U F R A X C I S C O
C.4LIF.
T H E writer has had iiunierous occasions to compare the Figure 1-Apparatus for Determination of Total Sulfur i n Natural-Gas Gasoline a n d Other Light Distillates
The results in Table I11 were obtained with a certain distillate by determining the total sulfur by the standard lamp method as described in U. S. Bureau of Mines, Technical Paper 298, page 48, and by the modified method here described.
-----
Table I11 SPECIFIC TOTAL SULFUR---2 3 .4verage GRAVITY 1 Per cent Per cent Per cent Per c e n t 0 314 0 314 0.311 0 76 0 317 Standardlamp 0 307 0 310 0 311 0 313 0 76 Modifiedlamp METHOD
The results in Table I11 are typical and indicate a satisfactory estimation of total sulfur by the moditied lamp method as compared with the standard lamp method. Crude Oil and the Heavier Distillates
The apparatus and manipulation for crude oil and the heavier distillates were the same as those described for natu-
viscosity of a batch of lacquer enamel in process of manufacture with that of a standard to be matched, where the opacity of the material rendered determinations by the bubble method highly unsatisfactory. The following modification of the bubble method proved satisfactory, and is nom used with good results. Two tubes are prepared, with the batch in process and the standard, respectively, just as they are for the bubble test. The heights of the liquid columns are adjusted so as to be equal, and the corks are inserted, not tightly, to the same depth into the tubes. The tubes are inverted and allowed to stand with corked ends down until the two bubbles are seen with equal clarity a t the upper ends. The tubes are then quickly and simultaneously inverted with one hand, while with the other hand both corks are simultaneously removed. The relative time required for each bubble to break through the surface of its liquid is a measure of the relative viscosities of the liquids. I
Received November 23, 1929.
