BRECKENRIDGE ON POTASH 1" E S T S I N A l I X E D F E R T I L I Z E R S . POTASH TESTS I N MIXED FERTILIZERS.' By J E. B R E C K E N R I D G E . Received J a n u a r y 15. 1909.
The conditions which the fertilizer chemist has to meet are hard to realize, unless one has had personal experience, as such. Especially is this true with regard to potash tests. On the one hand, the official methods, as outlined by the Association of Official Agricultural Chemists, must be followed and on the other hand we must satisfy the superintendents in finding the potash which they put into the goods. A brief account of the work of the Association of Official Agricultural Chemists during recent years, as reported in their proceedings, will give US some very interesting and profitable information. I n 1896 Messrs. Scoville, Peter and Curtis revealed the fact that it was necessary to use 300 cc. of water for making potash solution in order to prevent potash from being occluded in porous materials. Experiments were tried on filter paper and chamois skin and when small amounts of water were added to potash and these porous materials, the loss was 0.49 per cent, on 3.11 per cent. in case of filter paper and 0.40 per cent. in case of chamois skin. This loss was reduced to 0.03 per cent. by using 300 cc. of water and then making solution to 500 cc. and proceeding as usual. I t was also .found that when I O grams calcium phosphate were treated with I O cc. dilute sulphuric acid, boiled for onehalf hour, known amount of muriate of potash and water to 300 cc. added, then ammonia and ammonium oxalate and solution made to 503.5 cc., the 3.5 cc. accounting for the precipitate, that there was a loss of potash of 0.15 per cent. on 3.11 per cent. and 0 . 2 0 per cent. on 6.22 per cent. Conclusion.-Calcium phosphate precipitated carries down or occludes more potash than organic materials such as filter paper or chamois skin. The report for 1900 gives results of official method on acid phosphate and muriate mixture, showing the work of eleven experimenters. They found 6.12 per cent. K,O on 6.37 per cent. theory, a loss of 0.25 per cent. They found 3.07 per cent. K,O on 3.23 per cent. theory, a loss of 0.16per cent. Conclusion.-Low results on potash in Acid Phosphate and Potash mixtures, but lack of time prevented further work. rgor.---At suggestion of Mr. Carpenter, Mr. Hare, Read a t Meeting of American Chemical Society Dec. 31, 1908, Baltimore, Md.
409
referee, took up work of finding lost potash as experienced by official method. Results showed loss of 0.23 per cent. on 3 . 5 5 per cent. theory. Ammonium chlorid was tried as solvent for potash but gave only 0.07 per cent. increase in K,O. Conclusion.-- Further investigation into loss of potash by official method. 1902.--Mr. McDonnell, referee, reported loss of 0.43 per cent. K,O on 5.46 theory; when I O per cent. sulfate of potash and 90 per cent. acid phosphate were mixed together, about a 7 per cent. loss. On a mixture of 2 5 per cent. kainit, 40 per cent. acid phosphate, 20 per cent. blood and 15 per cent. fish, there was a loss of 0 . 2 0 per cent. on 3.11 per cent. theory, or about 7 per cent. Conclusion.-Further study of loss of potash by official method. 1903.-Mr. Carpenter, as referee, introduced the method of adding 5 cc. HC1 to 300 cc. water for making solution, adding soda in slight excess, then ammonium oxalate and proceeding as in the official method. Results showed 4.j6 per cent. on 4.55 per cent. theory on a sample of acid phosphate and muriate. Sample was also dissolved in regular citrate solution as used for insoluble phosphoric acid and only 0.10 per cent. was found insoluble in citrate solution as an average for ten workers, showing the potash found was a t least available. Mr. Carpenter also tried I O grams of sample of acid phosphate and potash boiled with 300 cc. water 112 hour, added ammonia and ammonium oxalate and filtered. Roiled residue with same amount of water, filtered and washed. Acid solution of resulting residue showed 0.30 per cent. K,O. j grams gave similar results. C o d mion.-Further investigation. rgog.--Under Mr. Carpenter, as referee, two samples were tried by the official method and Carpenter or modified method. Sample No. I . Acid phos. and muriate. Theory 4.31 per cent. K,O. Official method, 19 workers, average 0.41 per cent. low. Carpenter method, 19 workers, average 0.08 per cent. low. Sample No. 2 . Acid phos., animal tankage and muriate. Theory, 4.31 per cent. K,O. Official method, average 0.25 per cent low. Carpenter method, average 0.03 per cent. high.
T H E J O U R N A L OF I N D U S T R I A L A N D ENGINEERING C H E M I S T R Y . July, 1909
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We notice here that loss in acid phosphate and potash mixture is more than in acid phosphate, potash and tankage. This would seem to prove that the loss is caused by the acid phosphate and not increased by tankage as a n absorbent material. Mr. Carpenter recommended the adoption of the modified method, but it was decided to lay i t over until 1905. zgog.-Under G. S. Fraps potash work was done on three samples. No. 1 SAMPLE. ’
Acid phosphate and potash.
Theory 3.3491,.
................ 3 , 3 7 % ................ 2 ,927, ........ 0.4570 ........ 0.2670 .................. 3 . 6 2 % ...................3 . 17To . . . . . . . . . . . . . . . . 0.45% ........... 0.0670
Official method: Highest t e s t . . Lowest t e s t . . Difference. Average of all (6) 3.08% ; lo Modified method: Highest.. Lowest.. Difference.. Average of all (6) 3 . 2 8 % ; loss
No. 2 SAMPLE. Blood, acid phosphate and potash.
Theory 3.37% KzO.
.................... ............ ............ ............ Modified method: Highest.. .................. Lowest.. ................... Difference .................. Average 3 .27y0b;loss.. ....................... Official method: Highest..
3.1770 2.937, 0.24% 0 32% 3.42% 3 . l6y0 0,2670 0.10%
No. 3 SAMPLE. Cottonseed meal, acid phosphate and potash.
Theory 3.80%.
..................... 3 . 69Y0 ...................... 3.187’0 ................ 0 . 5 1 % ............... O.28Y0 Average of all 3 .52yc; 1 ............... 3 . 8 1 % Lowest.. . . . . . . . . . . . . . . . . . . . 3.6270 Difference.. ................ 0 . 1 9 % Official method: Highest. Lowest
Average of all 3 .7070; loss..
..................
0.10%
Again as in previous years we notice no apparent loss in complete goods over that in acid phosphate and potash. The acid phosphate seems to be the cause of the loss. The referee reported that “ we must conclude that the modified method gives results more nearly correct than does the official method.” The modified method was tried on some silicates with these results:
.................................. ........... .................. ................................... ............................... .......
Feldspar.. Microline. Leucite.. Apophyllite.. Muscovite 1.31-1.34 b y official method..
0 .OS% KzO 0.08% 0.3070 0.2770 0.91%
(From these results we see there is no danger of the modified method dissolving much more insoluble potash than the official method.) State fertilizer laws were discussed and i t was found 2 1 states required “ potash soluble in water” or “distilled water.” “ Law being made to exclude insoluble silicates,
i t might be argued that a method which does not include such potash and gives credit for the watersoluble potash placed in fertilizer, could be used.” Much discussion followed and when vote was taken the modified method was voted down. 1906 and 1907 added nothing of value as to finding lost potash, but the question of availability of potash was brought up by Messrs. Cushman & Bowker. No progress on available potash was made during these years nor in 1908, although it was decided in 1908 to appoint a special referee for available potash. Conclusions which may be drawn from work of Association of Official Agricultural Chemists during the past few years are : I . Loss of potash by official method in mixtures having acid phosphate and potash, this loss being in some cases as much as 7 per cent. 2. This loss does not seem to be increased by blood, tankage or cottonseed meal. 3. Laws of most of the states say “potash soluble in water,” consequently no acid can be used for solution as in the modified or ignition methods. 4. I n order to recover this potash and give the buyer a correct statement as to the potash contents, more work must be done trying to find method whereby water can still be used for solution and a cheniical added, perhaps, to hold this lost potash or the laws must say in place of “ potash soluble in water,” “ available potash’’ and leave it to the A. 0. A. C. to devise method for determining available potash. I n view of the fact that potash tests on mixtures having acid phosphate and potash are low, as obtained by the official method, this having been the experience of the -4. 0. A. C. and also the experience a t fertilizer factories, the following work has been done to locate this loss, if possible, and devise some method for finding this lost potash. A sample of acid phosphate and muriate was mixed in laboratorytand left on top of water oven for 24 hours. This sample No. I was carefully prepared and well mixed and methods I to IO, inclusive, used, for analysis. Method-No. I . Official method. No. 2 . Carpenter or modified method. No. 3. Dissolved sample in I per cent. citric acid solution by heating on steam bath for 40 minutes, added Na0.H in slight excess, then ammonium oxalate and proceeded as in official method.
BRECKENRIDGE ON POTASH T E S T S I N M I X E D F E R T I L I Z E R S . No. 4. Same as No. 3, only used 2 per cent. citric acid for solution. per cent. No. 5 . Same as No, 3, only used citric acid for solution. No. 6. Same as No. 3 , only used ammonia in place NaOH. No. 7. 2 0 grams in 300 cc. water, heated 40 minutes on steam bath, cooled, made up to 500 cc., filtered. Took 50 cc. filtrate, put into 2 0 0 cc. flask, added water to 150 cc., heated to boiling, added ammonia and am. oxalate and proceeded as in official method, evaporating 50 cc. equivalent to gram. No. 8. Same as No, 7, only added I gram citric acid to the aliquot in 200 cc. flask before adding ammonia and ammonium oxalate.
-
41 I
No. 14. Digested residue on filter from No. 11 in 2 0 cc. conc. HCl, evaporated excess of HC1, washed into 2 0 0 cc. flask, made to about 150 cc., boiled, added ammonia and ammonium oxalate and proceeded as in official method, giving us the potash insoluble in water but soluble in conc. HC1. From this series as shown in following table we find all methods for solution, except No. IO ( I per cent. am,), give decided increases over official method on sample No. I especially the No. 7 method, 2 0 grams in 500 cc. filtered, etc. This would seem to indicate that the insoluble residue when left in flask and ammonium oxalate 'added had an influence on giving low potash tests. The Carpenter and citric acid methods show well. Sample No. 2. Acid phosphate and potash.
TABLEOF POTASHRESULTS.
Methods. 1 Official. 2 Carpenter 3(a) Citric acid 1 per cent. 40 min. digestion, N a O H . . 3(b) Citric acid 1 per cent. 36 hours digestion, N a O H . . 4 Citric acid 2 per cent.. 5 Citric acid one-half per cent.. 6 Citric acid 1 per cent. plus ammonia.. 7 20 grams in 300 cc., e t c . . 8 Same as 7 plus citric a c i d . . 9 10 per cent. ammonia. 10 1 per cent. ammonia.. 11 2 grams on filter plus citric acid 12 2 grams on filter plus H C I . , 13 2 grams on filter.. 14 Insoluble on filter after washing Difference between 1 and 3 ( a ) in favor of 3 ( a ) . Difference between No. 1 and 13 in favor of 13.
m
N
.......................... 10.82 21.55 11.39 22.16 ............................................ ....... 11.12 22.03 ...... 11.11 .... ................................. 11.18 .... ........................... 11.24 . . . . ................... 11.18 .... .............................. 11.20 22.18 ............................. 11.22 22.24 ................................. 11.24 .... ................................. 10.69 .... ............. . . . . . . . . . ............................ ......... ................... ............. ..... 22.30 ..... 0.06 ............... 0 . 3 0 0.48 .............. ..... 0.75
......
No. 9. Used IO per cent. ammonia water for solution, heated 40 minutes on steam bath, added ammonium oxalate and then as in the official method.
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7 . 6 2 6 . 5 0 5.68 1.74 4.80 9.54 1.70 6 . 7 6 7.12 3.20 9.54 1.97 7.96 6 . 7 2 6 . 0 3 2 . 2 8 5.22 8 . 1 6 6.90 6 . 0 8 2.18 5 . 2 6 9.72 2.05 7.10 3.40 10.02
............ ............. .... ................................................. ................................................. ................................................. 8.16 6 . 9 3 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.91 6.96 5.70 1 . 6 0 4.65 9.32 1 . 5 6 7.02 6 . 6 4 3 . 1 8 9.54 .... 7.90 7.03 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5.58 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8.14 7 . 0 4 5.78 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 . 0 8 .... 6.04 1 . 6 6 4.78 .... 1 . 6 0 . . . . 6.92 .... 10.04 .... . . . . . . . . 6.02 1 . 7 8 4.78 .... 1.56 . . . . . . . . . . . . 10.16 .... 7.93 5 . 6 7 1 . 9 3 4.80 9 . 8 8 1 . 5 6 6.92 6 . 9 6 3 . 1 0 9 . 8 .... 0 . 0 2 0 . 8 1 0.54 . . . . 0 . 4 8 . . . . 0 . 0 8 0 . 5 0 . . . 0.54 0 . 4 0 0.40 0.44 0 . 4 6 0 . 1 8 0 . 3 5 0 . 3 4 0 . 0 8 0.20 0 . 4 8 . . . . 0 . 3 1 0 . 3 8 .... 0 . 1 9 . . . . 0.34 . . . . 0 . 1 6 . . . . . . . . 0.34 ....
This was taken from stock in factory about three months old. Results on this were:
.
Method No. 1 . . ' I " 2... ,, (L 3... I , I' 7.. " " 8.. , 13,.
21 .SO-21 .60% Difference. Official method 22.1670 0.61yo Carpentermethod. 22.0370 0,4870 citricmethod 22.1870 0.6370 water-soluble method 2 2 .24y0 0 69y0 water citric method 2 2 ,30% + grams on filter
+
Used I per cent. ammonia water for + solution, otherwise as in No. 9. . + + + No. I I . Placed 2 grams on I I cm. filter, washed . with hot water, small portions a t a time, into 2 0 0 Here again we find the official method very low CC. flask to about I 7 5 CC., when there should be no and No. 7 showing fine, Carpenter and citric also chlorine or soluble sulfate left in residue, add to showing fine, 2 grams on filter showing best. filtrate about 0.6 gram citric acid, heated to boiling, SAMPLENo. 3 5-8-8 GOODS. added ammonia and ammonium oxalate. then as in Method NO. 1 . . . 7 . a % Difference. Official method ." ', 2 . . . 7.96% + 0 .347c Carpenter method the official method, evaporating 5 0 cc. = :b gram. 3... 8.16yo + 0.54Tc citric + soda '' 6 . . . 8 . 1 6 % + 0.54yo citric + ammonia No. 12. Same as No. I I , only using z cc. HC1 7. , . 7.91% + 0.29'% water-soluble conc. in place of 0.6 gram citric acid. . 8.. 7.90% + 0.2870 water-soluble + citric acid NO.13. Same as NO, 11, omitting 0.6 gram '' 1 4 % + 0.52% 1% ammonia ,, 1I O1 .... .. 88 ..OS% + 0.46% 2 grams on filter + citric acid citric acid. " 1 3 ... 7.93% + 0 . 3 1 ' % 2 g r a m s o n f i l t e r
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412
Again the official method is lowest, Carpenter and citric acid showing best, while I per cent. am. sol. method No. IO shows fine. No. 7 , No. 1 1 and No. 13 also show good gains.
the greatest influence on the lost potash. To further prove that the potash in usual acid phosphate and potash mixtures goes into solution readily and is lost in process, I took 2 grams of SAMPLENo. 4 4-8-7. sample NO. 2 , acid phosphate and muriate testing Method No. 1 . . . 6.50% Difference. Official method 21.55 per cent. by the official method, placed on 2... 6 . 7 2 % + 0 . 2 2 % Carpenter 1 1 cm. filter and washed with sinall portions of 3... 6 . 9 0 % + 0 ,407' citric 6.9370 + 0 .43Y0 citric and ammonia " 6... hot water to 175 cc. in zoo cc. flask, the washings " 7 ... 6 . 9 6 % + O.46Y0 water-soluble no longer showing any chlorine, treated the residue 7 . 0 3 % + 0 . 5 3 % water-soluble + citric 8... 7.04% + 0 . 5 4 % 1% ammonia (' 10 . . . with 2 0 cc. conc. HC1 evaporating to T O cc. washed 6 . 8 8 % + 0.389'0 2 grams on filter 13.. . into flask, boiled, added ammonia and ammonium Again the official method shows lowest, oxalate and proceeded as in the official method SAMPLE No. 5 3-6-6. (method No. 14) and found 0.06 per cent. K,O. Method No. 1 . . . 5 .68Y0 Difference The water solution was analyzed by regular official " 2... 6.0370 + 0.359'0 3... 6.08y0 + 0.4070 method and showed 2 2 . 3 0 per cent. K,O against 7... 5 . 6 7 % - 0.0170 2 1 . 5 5 K,O by the official method as usually carried 5.58% - o.10yo '( " 9. . . lo... 5.76% + 0.08% out. 6 . 0 4 y 0 + 0.36v0 " 1 1 ... Sample No. 6 3-6-6 was analyzed for insoluble 12.. . 6 . 0 3 7 0 + 0.35y0 potash by washing on filter as on sample No. 2 Again methods Nos. 2 , 3 , I I and 1 2 show decided and residue treated with conc. HC1 and proceeded gain while water solution and ammonium solution as before (method No. 14) and found 0.02 per cent, show low. I n this sample we find the loss of potash in the Sample No. 6 10-2. process after removing the insoluble material SAMPLENo. 6 1 0 - 2 . probably due to the fact that there were more Method No. 1 . . . 1 .74% Difference 2 . 2 8 7 ? + o.54yo 2... soluble salts, precipitated by the ammonia and 2.1sy0 + o,44yo 3... ammonium oxalate, in this sample than in the 1.607' -0,14'% 7... 1.930/, + 0 . 1 9 % 13 . . . samples No. 2 (5-8-8) and No. 3 (4-8-7). Again the Carpenter (No. 2) and citric (No. 3 ) Methods No. 1 1 and No. 1 2 were tried on 3-6-6 methods show all right while i t seems that No, 7 and potash was found. The tabulated results boiling with water and filtering lost a little. No, 13 will show the work done and the conclusions which shows well. can be drawn are : To try to locate where this loss occurred I made I . That the official method gives low results. the following rests: 2 . That the potash found by the Carpenter and I . Acid phosphate known amount of muriate citric acid methods in samples No. z and No. 3 in solution, then the official method showed a loss a t least, is not insoluble potash, as shown by anof 0.32 per cent. on 6 . 4 4 per cent. alyzing the insoluble residue after washing with hot 2 . Acid phosphate water NaOH in excess water. am. oxalate, to precipitate all the lime before 3. That filtering off the insoluble residue in some adding the potash, then added known amount of cases gives us higher results than the official method. potash and proceeded as in official method gave 4. That while I believe the law should read still a loss of 0.27 per cent. and 0 . 2 1 per cent. on " available potash" and so permit the use of HC1, 6 . 4 4 per cent. or a t least citric acid for solution, and recover the From this i t would seem that the precipitate or potash which was added as soluble but has probably insoluble material, or both, usually found in potash formed zeolites as in samples No. 6, No. 7 , No. 9 determinations, when solution has been made and No. 1 2 , under the existing laws we are comalkaline and am. oxalate added, takes up potash pelled to use water for solution. Satisfying this in some way and that it is not necessarily the pre- condition, method No. 7 , 20 grams in 3 0 0 cc. water, cipitation that causes the loss. I n fact our ex- etc., gives us a decided increase in potash over the perience with method No. ;, filtering off the in- official method on some samples and loss in others. soluble material, would seem to indicate that this Method No. 1 3 gives decided increase over method insoluble material, calcium sulfate, silicates, di- No. 7 on samples No. 8 and No. 13 with equally calcic phosphate being a part of this insoluble, had good results on others. Methods No. 1 1 and No. "
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E M M E T T A N D G R I N D L E Y O N C H E M I S T R Y OF F L E S H . 1 2 give decided increases on samples No. 5 and No. 13 and will recover potash in many cases where the official method loses it. I,ABORATORY A M E R I C A N AGRICULTURAL C H E M I C A L
CO.,
CARTERET, N. J.
CHEMISTRY OF FLESH. (SEVENTH PAPER.)
A PRELIMINARY STUDY OF THE EFFECT OF COLD STORAGE UPON BEEF AND POULTRY. (FIRST COMMUNICATION.) B y A. D . EMMETT A N D H. S. GRINDLEY. Received March 10, 1909.
U p to the present time, the modern method of cold storage must be considered as the best means of preserving flesh from the standpoint of supplying a product which closely resembles the freshly killed meats. Further, i t gives a safe and convenient medium wherein the physico-chemical changes of fresh meats can take place, as for example, rigor mortis which may occur almost immediately after death, later giving way to release rigor and thereby causing the flesh to become softer and more tender. Further in the continued hanging of the meats, they are supposed to become juicier, better in flavor and tenderer, or in the trade sense ripened and in prime condition for domestic use. Naturally, the influence of the factor of time of keeping meats in cold storage is an interesting one, especially if we consider the transportation of meat products both a t home and abroad. During a cold storage transit period of 2 2 days, the time required to go from Argentina to England, or of 40 days, the time to‘go from Australia to England, i t would be instructive and perhaps of economic value to know more of the chemical changes which take place in the stored meats during transit, Whether cold storage influences the nutritive value of the food stuff, appreciably affecting its palatability or its comestibility, and if so an approximation as to the time when the changes take place would add to our present knowledge. Another factor which is also of interest a t the present time is the effect of cold storage upon frozen fowl, whether the drawn or undrawn bird is preserved equally well for the same length of time, and what are the differences, if any, in nutritive value in the two cases as compared with fresh fowl.
With the object of making a chemical study of the influence of cold storage upon flesh, this investigation was undertaken. The present paper, which takes up the preliminary work in applying the improved methods of analyzing flesh,‘ to fresh arid refrigerated products, deals as nearly as possible with the existing conditions first, as they relate to the storage of chilled or refrigerated beef for periods of time which may be counted as comparable to those required to ship and transport our products to their destination, and second to the storage of drawn and undrawn frozen fowl. I n the meantime, W. D. Richardson2has applied the methods to a study of the deterioration and commercial preservation of flesh foods, and has proved that they are of real value in this connection. H. W. Wiley3 has also used our improved methods for the analysis of flesh in his study of the effects of cold storage upon poultry. HISTORICAL.
Among the investigators who have studied the effect of cold upon meats, may be mentioned Bouley4 who in 1874 presented a paper before the French Academy of Science. He stated, in using Tellier’s process of refrigeration, that a t a temperature between t-3’ C. and - 2 O C. meat would keep indefinitely as far as putrescibility was concerned b u t not so from the standpoint of an edible food, for while the tenderness of the meat was increased with the time of storage a peculiar fatty odor developed toward the end of the second month which affected the flavor. Pogziale and a little later, in 1889, a commission appointed by the French minister of war confirmed Bouley’s conclusions. In 1892, Grassmans found in making a study of beef, pork, and mutton: that flesh kept in cold storage for 8 months a t -2’ to -4’ C. did not deteriorate; that considered upon the dry basis the data indicated that there was no loss of nutritive material, this statement being based upon the following chemical determinations, moisture, total nitrogen, protein nitrogen by Stutzer’s method, and f a t ; that refrigerated meats cook by roasting and boiling in a shorter time than do the fresh 1
Grindley and Emmett, Journ. A m e r . Chem. Sac., xxvii. 658-678 Emmett and Grindley, I b i d . , xxviii, 25-63, (1906). Journ. Amer. Chem. S o c . , 3 0 , 1515-1564 (1908); THIS JOURNAL,
(1905). 2
H . S. Grindley, Journ. of the Amer. Chem. S o c . . x x v i , p . 1086 (1904); H . S. Grindley and A. D. Emmett, Ibid., xxvii, p . 658 (1905); A. D . Emmett and H . S. Grindley, I b i d . , xxviii, p , 25 (1905); P. F. Trowbridge and € I, S. Grindley. I b i d . . xxviii, p. 469 (1906); H . S. Grindley and H . S . Woods, Journ. o j B i d . Chem., 2 , p . 309 (1907); A. D . Emmett and H. S. Grindley, I b i d . . iii, p. 491 (1907).
4’3
1, 95-102. 3 “A Preliminary Study of the Effects of Cold Storage on Eggs, Quail, and Chickens,” U .S. Degartment of Agricullure, Bur. of Chem.,
Bu12. 115 4
(1908).
Comfit. rend., 79. Lamdw. Jahrb., 21.
