potassium and sodium, washing the filter and contents, and precipitating the calcium out of the filtrate in the ordinary way with ammonia and ammonium oxalate.

Total neutral fat and unsaponifiable matter.-To determine these two substances, about 10 grams of the soap is weighed out and dissolved in alcohol. Fifty to 70 grams of acid washed, ignited sand is now added and the alcohol evaporated off. The mass is dried and transferred to a Soxhlet extractor, where it is extracted with ether. This extract contains neutral fat, unsaponifiable matter, and free fatty acids, which are weighed together. The free fatty acids are determined by means of standard alkali and phenol phthalein and subtracted from the other two.

Resin acids. A rather large quantity of the soap is first dissolved in water and, after heating to boiling, enough dilute hydrochloric acid is added to set the fatty and resin acids free. The boiling is continued till the fat collects in oily drops. The vessel is cooled and the acid water poured off. The residue is again boiled with water, which is again poured off. The fatty matter now remaining is washed with cold water and transferred on a watch glass to a desiccator, where it is thoroughly dried. The resin acids are determined in a weighed quantity of this mixture by the Twitchell method. For this dissolve 2 or 3 grams of the mixture of acids prepared as above and place in a flask in about 10 times their volume of absolute alcohol. Pass a current of dry hydrochloric acid gas through the flask, which is immersed in ice water. Pass the hydrochloric acid through for about threequarters of an hour, or until it is noticed that the gas is passing through the liquid unabsorbed. Set the loosely covered flask aside for one hour, dilute with 5 volumes of water, and boil until the water layer becomes clear. Transfer to a separatory funnel, washing out all the ethylic ethers and resin acids with ether. Shake well and run off the acid layer. Wash the etherial solution a number of times with pure water until all hydrochloric acid is removed. Now add 50 cc of alcohol and titrate the solution with standard potassium hydroxid, using phenol phthalein as indicator. The resin acids combine with the alkali and the ethylic ethers are practically not touched. To obtain the amount of resin, multiply the number of cc of normal alkali used by 0.346. One hundred parts of resin acids are equal to 97.32 parts of resin anhydrid.

ANALYSES AND DISCUSSION.

The table following (IV) shows the composition of various soaps:

19557... Whale-oil Soap, Per et. Per ct. Per ct. Per ct. Per ct. Per ct. Per ct. Per ct.

Free caustic alkali.

Per cent. Acid reaction.

"Lion Brand

5.82

86.38

20455... Whale-oil Soap

204560..

.do..

20458a.. Permol Kerosene

Soap

20459... Whale-oil Soap

20460... J. & M. Reliable

Insecticide.

20461... Stott's Fir Tree

Soap.

9 I& W

20696... Insecticide from
Florida
Lemon-oil Insecti-

20458. The greater part of the unsaponifiable matter in this sample on being subjected to distillation distills over between 300° to 400° C., and is evidently composed of the higher boiling products of petroleum.

20460. It appears that one alkali is present in the fatty acid soap, and another has been used to saponify the resin.

20461. The unsaponifiable portion of this sample appears to consist of products from either the fir or pine, and closely resembles turpentine. Low results were obtained doubtless because some of the unsaponifiable matter was volatile with water.

9 I. & W. The fatty acids are mixed to quite a large extent with resin or resin oil. lemon oil, it is extremely doubtful, as its presence is not shown.

If there is any

The soaps sold under the name of "Whale-oil soaps" are usually not really whale oil, but are made of some cheap fish oil. Marlatt" says in regard to such soaps that they are especially valuable in destroying soft-bodied insects. He further remarks that a soap should be demanded which is made with potash rather than soda, since the former is more effective and more readily sprayed, and that not more than 30 per cent of water should be present. The figures for the whale-oil soaps in Table IV show that none come in this classification. While soaps 19557, 20455, 20457, and 20459 contain only a moderate amount of water, they are in every case hard or soda soaps. The only whale-oil soap that is soft and contains potash is 20456, and this contains entirely too much water.

Permol Kerosene Soap appears to consist of about 10 per cent moisture, 35 per cent soap, and 53 per cent crude petroleum products, especially paraffin. It will doubtless have the same good effect as the usual soap-petroleum emulsion.

J. & M. Reliable Insecticide is the well-known resin soap, containing in this case about 36 per cent resin soap, 27 per cent fatty acid

a Farmers' Bul. 127, U. S. Department of Agriculture.

soap, and 34.30 per cent moisture. The merits of a resin, fatty acid soap mixture are well-known and so do not need repetition.

Stott's Fir Tree Soap evidently consists of a mixture of fatty acid soap and some fir or pine tree products. It may serve the purposes for which it is intended but has not been tested to the author's knowledge. Sample No. 20696 is an insecticide forwarded from Florida by a private party through the Entomologist of the Department. It evidently consists of a mixture of resin soap and fatty acid soap dissolved in water. It has the advantage of having potash instead of soda as the alkaline principle, and will doubtless serve the purpose for which it is intended. A small amount of alkali is in the free condition, but hardly enough to injure the foliage.

Lemon-oil Insecticide is evidently a water solution of resin and fatty acid soap, with potash as the alkaline principle. Its name is misleading, in that we would expect to have some lemon oil present. Twentyfive cents per pint is a rather high price for such a mixture.

HELLEBORES.

The roots of Veratrum viride, or American hellebore, and the roots of Veratrum album, or European hellebore, when ground in a powder possess considerable insecticidal qualities.

In making an analysis of this class of compounds, a determination of the following constituents was made: Moisture, ash, to see if the roots had been properly freed of dirt, and alkaloids present, to see if they were the alkaloids that should be present in true hellebore roots.

METHODS OF ANALYSIS AND DISCUSSION.

Moisture.-Dry 1 to 2 grams of the sample at the temperature of boiling water for 12 to 14 hours. The loss in weight is reported as moisture.

Ash.-Burn the dried sample from the above determination at a low red heat to a white ash. The residue is reported as ash.

Alkaloids. From Veratrum viride" 6 well-defined alkaloids have been extracted, namely, jervine, pseudojervine, rubijervine, veratralbine, veratrine, and cevadine. All of these except cevadine are also present in Veratrum album. In extracting and testing the above samples, the following method is followed: The finely powdered substance is extracted for 3 to 4 hours with water weakly acidified with sulphuric acid at a temperature of 40° to 50° C. It is then filtered through a folded filter and the filtrate transferred to a separatory funnel. It is first extracted in the separatory funnel with petroleum ether to get rid of coloring matter, etc. It is then extracted with chloroform.

@ See Wright and Luff, Jour. Chem. Soc., 35, p. 401–426.
See "Poisons: Their Effect and Detection," 3d ed., Blyth.

This extraction with chloroform is repeated a number of times, thus extracting most of the alkaloids of hellebore, either partially or wholly. This solution, which we will call A, is put aside, and the contents of the separatory funnel is made alkaline with ammonia and extracted with petroleum ether to obtain any alkaloids that are left, particularly veratrine, making solution B.

Portions of solution A are placed in watch glasses, allowed to evaporate spontaneously, and finally tested with concentrated sulphuric acid. On employing two samples known to be pure, the following results are obtained: The residue left is amorphous. On treating it with a drop of sulphuric acid a yellow solution is first formed, changing to brown, then purplish red on the edges, and finally, after standing about half an hour, purplish red throughout the whole mass. Portions of B are now treated in the same way, and on two pure samples the following results are obtained: The residue is amorphous. On being treated with concentrated sulphuric acid a yellow solution first forms, which turns dark yellow, chestnut, and finally brown red, with sometimes a greenish color around the edges of the drop."

Of course, there are some substances that might give the same play of colors with sulphuric acid as those described, but probably not any that would likely be used to cheapen the product.

ANALYSES AND DISCUSSION.

The results obtained by the above methods of analysis are given in the following table:

a According to Allen's Commercial Organic Analysis, the pure alkaloids should give the following play of colors with concentrated sulphuric acid:

Jervine: Yellow, brown yellow, bright green.

Pseudojervine: Yellow, bright green.

Rubijervine: Yellow, orange, dark red.

Veratralbine: Yellow, orange red, blood red with green fluorescence.

Veratrine: Exactly like cevadine except that the red solutiou is not fluorescent.

Cevadine: Yellow, brown red, blood red with greenish fluorescence; if allowed to stand in air long enough, becomes purple.

A glance at the moisture figures in Table V shows that the variation in the 9 samples is not very great, with a minimum of 6.23 per cent and a maximum of 8.87 per cent.

As to the percentage of ash, it must be remembered that these preparations are the powdered root of a plant. We would therefore expect to find a rather high ash content, which would be much increased if the roots had not been properly cleansed. The figures show that there is at any rate no reason that the ash content should be above 15 per cent, and evidently, with proper handling, this can be very much reduced. Adopting, then, 15 per cent as the maximum amount allowable, it will be seen that samples 19836 and 19837 are very much above this limit, and 19558 slightly above.

Since the alkaloidal principles in the above 9 samples, on being treated with concentrated sulphuric acid, act exactly similar to the alkaloidal principles of 2 samples known to be pure, and also follow fairly closely the color changes as indicated for the alkaloids of the hellebores in chemical literature, these samples appear to belong to the class of hellebores. The color changes seem to follow most closely those indicated for cevadine, which might be expected if the above samples are roots of Veratrum viride, since this alkaloid appears in quantities greater than the sum of all the other alkaloids.

PYRETHRUMS.

The next group of substances to be taken up are the pyrethrums, which include Pyrethrum roseum, or Persian Insect Powder, and Pyrethrum cinerariæ folium, or Dalmatian Insect Powder, and Buhach.

The ground flower heads of these plants are used to kill insects. Such preparations contain as their active principle a volatile oil, which quickly oxidizes on exposure to the air to an inactive resin." This oil may be determined by extracting with ether and drying at a low heat. Four samples examined by Hilgard gave the following results:

Such powders sometimes contain either lead chromate, barium chromate, or tumeric, to give them a bright yellow color or to palm off some entirely different powder as one of the pyrethrums.

METHODS OF ANALYSIS AND DISCUSSION.

In making an analysis of these products the following determinations were made: Moisture, ash (a large amount of which indicates the

a Hilgard. Report of the College of Agri. Univ. of California, 1879, p. 68.