Two grams of the ash were first fused with sodium carbonate and the fused mass washed with water containing sodium carbonate. The residue was washed into a beaker and treated with a few drops of sulphuric acid. The residue now remaining was filtered and after ignition was treated with hydrofluoric and sulphuric acids. After evaporating off these acids, the residue was treated with sulphuric acid water, filtered, and then fused with sodium carbonate. After extracting with sodium carbonate water, the residue was dissolved in just enough hydrochloric acid and precipitated with sulphuric acid. The precipitate was dissolved in concentrated sulphuric acid and reprecipitated by water and weighed as BaSO_{4}. So far as the writer can ascertain, there have been no control experiments made for this method to determine the experimental error.
Of the above ash, 1.998 grams gave 5.2 milligrams of BaSO{4}, which would correspond to 75.75 milligrams of barium acetate crystals-- Ba(C{2}H{3}O{2}){2}+H{2}O--in 200 grams of the dried plant. The residue by the Hillebrand method after weighing was tested with the spectroscope and gave a bright spectrum for barium. The same ash was analyzed by the Bureau of Chemistry, using a shorter method, and they reported 2.7 milligrams of barium sulphate in 1.1217 grams of ash. A second sample collected earlier in the summer, with an ash content of 18.6 per cent, was shown to yield barium corresponding to 3.4 milligrams of BaSO_{4} in 2.5 grams of the ash.
One lot of Aragallus lamberti collected at Hugo, Colo., in May, 1905, and which gave an ash content of 37.3 per cent, was found to yield 3 milligrams of BaSO{4} from 1.998 grams of ash, or 173.88 milligrams of Ba(C{2}H{3}O{2}){2}+H{2}O in 200 grams of the dried plant, but this ash also contained 0.27 per cent of SO{3}. The Bureau of Chemistry reported the barium to correspond to 2.9 milligrams of BaSO{4} in 2.45 grams of the ash.
The Astragalus missouriensis (Hugo, June, 1907), with an ash content of 21.8 per cent, gave 3 milligrams of BaSO{4} in 2.01 grams of ash, or 76.58 milligrams of Ba(C{2}H{3}O{2}){2}+H{2}O in 200 grams of the dried plant. The residue after weighing was tested spectroscopically and gave a bright barium spectrum.
The Astragalus drummondii from Custer, S. Dak. (1906), Astragalus mollissimus from Kit Carson County, Colo. (December, 1906), and Astragalus nitidus from Woodland Park, Colo. (October, 1907), were reported by the Bureau of Chemistry to contain no barium.
The ash of the Astragalus pectinatus (Hugo, June, 1907) was reported by the Bureau of Chemistry to show no barium on spectroscopic examination.
Two grams of active loco plant ash yielded from 5 to 6 milligrams of BaSO_{4}, but it can be easily seen that in multiplying this amount to correspond to 200 grams of the dried plant errors would be likely to arise, so that the whole amount of barium would not necessarily be accounted for.
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FOOTNOTES:
Hillebrand, W. F. Analysis of Silicate and Carbonate Rocks. U. S. Geol. Surv. Bul. 305, p. 116. 1907. See also Folin, O., On the Reduction of Barium Sulphate in Ordinary Gravimetric Determinations, in Journ. Biol. Chem., vol. 3, p. 81. 1907.
All the determinations of barium which resulted either positively or negatively were made with the same bottle of sodium carbonate and H{2}SO{4}, so that impurities in the chemicals were thus eliminated.
Report from Bureau of Chemistry.
=ANALYSIS OF SOILS.=
One sample of the soil from near Hugo, Colo., from which the Aragallus lamberti was collected, was examined by the Bureau of Soils, and that Bureau reported the absence of barium and zirconium, at least of any recognizable by the chemical methods used, so that it can not be said that the barium came from any soil accidentally mixed with the ash. Traces of titanium were, however, found. Evidently the plant must collect minimal quantities of these elements from the soil and store them.
The water from a well of an adjacent area was examined by the Bureau of Chemistry and reported to contain 37.4 parts of calcium and 13.7 parts of magnesium in one million, and that the water contained no barium.
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FOOTNOTES:
Barium has been found in well water in England. See Thorpe, T. E., Contribution to the History of the Old Sulphur Well, Harrogate, in Philos. Mag., 5 s., vol. 2, p. 50, 1876.
=FEEDING EXPERIMENTS WITH BARIUM SALTS ON ANIMALS IN THE LABORATORY.=
On these figures the writer took 0.2 gram of crystallized barium acetate c. p., using the acetate because acetic acid has been proved in certain loco plants by Power and Cambier, and after dissolving it in water fed it at 9.45 a.m. to a rabbit weighing 1,177 grams. The head soon fell forward so that the nose rested on the ground. At 10.58 a.m. the rabbit seemed unable to guide itself and would run into obstructions if forced to move. There was no diarrhea but it urinated several times. There was a peculiar tremor of the muscles noted. The animal would not startle by sudden noises and at 11.06 a.m. could be placed on its back with ease. The pupils appeared about normal. The whites of the eyes showed very prominently. At 11.35 a.m. the fore legs were paralyzed. The following morning the animal was dead, its weight being 1,120 grams. The heart was dilated; the stomach was not hemorrhagic, but rather pale.
A second rabbit, which weighed 1,630 grams, was fed with a solution of 0.5 gram of the same salt at 9.42 a.m. At 10.35 a.m. the animal passed soft stools and showed a marked disinclination to move, with evidence of pain. The diarrhea became more marked and the animal's hind quarters were soiled with feces. At 10.48 a.m. there was marked incoordination of the limbs and inability to stand. Finally, at 10.56 a. m., convulsions began and the animal died at 11.02 a.m. The autopsy was made about two hours later. The animal was then rigid. The kidneys seemed rather congested. The intestines were relaxed; mesenteric vessels dilated. The pyloric region of the stomach appeared hemorrhagic.
A third rabbit, fed like the preceding with 0.5 gram of barium acetate, showed much the same result. In this case there was some retching, but the other symptoms were as above, the animal dying in one hour and five minutes. No hemorrhages were seen in the stomach walls. It was noted that after the administration of certain doses, 0.2 gram, there was no diarrhea.
On September 23, 1907, a rabbit weighing 1,757 grams was fed at 10.42 a. m. with 0.1 gram of the same barium acetate. The temperature at the time of feeding was 102.9°F. At 12.05 a.m. the animal urinated. Temperature, 101.4°F. On September 24 the animal weighed the same. Temperature at 10.55 a.m., 102.3°F. The same amount of barium was fed. At 3.40 p.m. the temperature was 102.5°F. On September 25 the animal weighed 1,800 grams. Temperature, 102.2°F. at 10.39 a.m. The dose of barium was repeated. At 3.55 p.m. the temperature was 101.4°F. On September 26 at 9.38 a.m. the temperature was 101.1°F., and again the barium was given. At 3.57 p.m. the temperature was 101.5°F. On September 27 the rabbit weighed 1,772 grams. The temperature at 9.53 a. m. was 102.3°F. The barium was fed for the fifth time. At 10.27 a.m. there were general convulsions. The eyes teared. At 10.32 a.m. soft stools appeared and the animal urinated. Stools were passed at various periods. At 11.30 a.m. there were no signs of pain on pinching the ear. At 11.58 a.m. the animal retched. The animal was lying with the fore legs wide apart and could not support itself. At 12.05 p.m. the temperature was 98°F. and the rabbit died shortly after.
The peritoneal cavity seemed normal. The small intestines were relaxed, while the mesenteric vessels were dilated. The kidneys seemed congested. The stomach walls were pink and in places covered with mucus. The heart was relaxed save the left ventricle, which seemed firm.
On September 23, 1907, a second rabbit, weighing 1,360 grams, was fed with a similar solution and the feeding was repeated at the same time the first rabbit was fed. On September 27 the animal weighed 1,416 grams. On this day a peculiar movement of the hind legs on jumping appeared, apparently due to an inability to draw the legs completely up, and the fore legs were spread wide apart, as if too weak to support the animal. The temperature had also fallen. On September 28 the animal had apparently recovered. Weight, 1,516 grams on October 21.
On September 23, 1907, a third rabbit, weighing 1,304 grams, was fed with 50 milligrams of barium acetate. This dose was repeated each time the other two rabbits were fed. On September 27 it weighed 1,304 grams. Marked muscular twitching appeared, with disinclination to move. Finally there were convulsions and paralysis of the limbs. No stools were seen. This animal lay quiet all night, apparently unable to move, and continued on its side until 3.15 p.m. on September 28, when it gradually recovered, weighing 1,346 grams on October 24.
On October 24, 1907, a rabbit weighing 1,346.5 grams was fed with a solution of 25 milligrams of crystallized barium acetate. On the next day the weight was 1,318 grams, and the dose was repeated. On October 26 it weighed 1,275.7 grams, and the dose was repeated; on October 30 it weighed 1,332 grams, and on October 31 its weight was 1,375 grams. The animal died at night on November 6; weight, 1,134 grams. The post-mortem examination, made with Dr. Meade Bolton, of the Bureau of Animal Industry, was negative save for the presence of necrotic tissue in one enlarged thyroid.
On October 24, 1907, a rabbit weighing 1,332 grams was fed with a solution of 25 milligrams of crystallized barium acetate. On the next day the animal weighed the same, and the dose was repeated. On October 26 it weighed 1,289 grams, and the same amount of barium was given. On October 28 the weight was 1,219 grams and two days later 1,289 grams.
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