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On the detection of cotton-seed oil in lard |
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Analyst,
Volume 13,
Issue 9,
1888,
Page 161-165
Alfred H. Allen,
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摘要:
THE ANALYST. SEPTEMBER, 1888. __ ~ __ ON THE DETECTION OF COTTON-SEED OIL I N LARD. BY ALFRED H. ALLEN. (Read at Meeting, Jzcnt3, 1888.) I HAVE recently had occasion to look into the question of the adulteration of lard with cotton-seed oil, and for the purpose of comparison have analysed certain samples, known162 THE ANALYST. Solidifying point ; O C . . . . . . . . . . . . . . and suspected to be adulterated, together with certain specimens of which the genuine nature was beyond suspicion. The figures given by the lwd marked '' Zlmentum " were yielded by a specimen rendered in my laboratory :- The following table shows some of the results obtained. $ ,(Melting point ; O C . . . . . . . . . . . . . . . . t+ I Solidifying point; "C . . . . . . . . . . . . . . 2 I Plummet gravity at 99°C .. . . . . . . . . 8 (Iodine absorption, per cent. . . . . . . . . Omen- turn Lard. 39.0 26-5 rising to 27.5 *8602 55.4 39.0 38.7 rising '0 39.0 -8372 274.5 58.3 58.4 87.4 white Leaf Lard. 40.0 32.0 ~8620 60.5 39.5 38.5 rising ;o 38.8 ,8385 65.3 white 37.5 27.6 8648 82.5 Markec ening black. 40.0 30.5 -8637 68-8 39.5 373 rising to 38.5 -8450 276 8 70.4 57.8 (94.6) Markec black. ening -8628 62.8 ,8385 64.8 lensible dark- ening. The following Ggures are the recorded results of experience with tallow, lard, and cotton-seed oil :-- 2 (Melting point; "C . . . . . . . . . . . . 0 R & Solidifying point; "C . . . . . . . . . . . (Iodine absorption, per cent . . . . . . . 2 ? Specific gravity at 9 9 " ~ ' . . . . . . . . Melting point ; "C . . .. . . . . . . . . . Solidifying point ; "C . . . . . . . . . . . Specific gravity at 99OC . . . . . . . . . (Iodine absorption, per cent.. . . . . . Tallow. 33- 48 a862 40 45 43 41.3 - Lard. 28-45 .860--.8 6 1 59-62 38 38 64.2 - Jotton-seed Oil. flnid -872 1 0%- 1 1 0 35-36 30 846.7 115.7 I n addition to these Muller has recorded the following iodine-absorptions :-Beef- suet, 38.4 ; lard, 55.0 ; cotton-seed oil, 107.9.THE ANALYST. 163 Mr. J. Carter Bell informs me that he recently found 51.5 as the iodine-absorp- tion of a sample of leaf-lard which he prepared himself. The same sample yielded 51.2 in the hands of Mr. R. Williams, while Mr. E. W. T. Jones found 46.57. I have this day received from Mr. Chas. M. Blades a sample of cotton-seed stearin, which is now a commercial product.I have attempted in vain to obtain this article for years past, in consequence of the result recorded by Dr. Muter (ANALYST, vii., 93), who described the adulteration of lard with this product. The ordinary cotton-seed stearin of commerce is really the stearic acid from cotton-seed oil, and quite a different article from the sample of neutral fat now before you. The figures given in the following table, in the column headed " Cotton-seed Fat," are those yielded by the sample in question :- (1 Fat. I Oil. 1 from B. Plummet gravity Melting point. . , Solidifying point s t 99%. ............... ....................... ...................... Iodine absorption ...................... Saponification equivalent ................ Acidity ( = Oleic Acid).................. 08684 4OoC 31 rising to 32.50 89.8 -34 - *8725 - 108-1 10 285-294 trace 08476 35OC 3 2 O 115.8 289% 97.6 The results I have obtained substantially confirm those of Mr. Jones, Mr. Rowland Williams, and other previous observers, and appear to show that lard differs materially in its iodine-absorption from beef-stearin on the one side and cotton-seed oil on the other. There is also a marked difference in the specific gravity of lard and cotton-seed oil, and this difference is also noticeable in the fatty acids. On the other hand, lard and beef-fat are substantially of the same density. This difference is very important, as it would enable one to distinguish a mixture of beef-stearin and cotton-seed oil, having an iodine-absorption of about 60, from genuine lard.Thus, while the proportion of the adulterant in a mixture composed of lard and cotton-seed oil only can be ascertained with considerable accuracy by determining the iodine-absorption, the estimation will be below the truth if beef-stearin be present. On the other hand, the presence of beef-stearin does not interfere with the deduction to be drawn from the increased specific gravity of the melted sample. Hence this method, though not affording more than approxi- * Mr. Rowland Williams, in his recent paper on the characters of certain fatty acids (ANALYST, xiii., SO), quotes '' other observers as recording a range of 275 to 337 for the mean combining weight of the fatty acids from cotton-seed oil." On reference, I found, to my surprise, that the anomalous figure 337.2 was one recorded by myself.I feel sure this figure is erroneous, though I am unable, at this distance of time, to ascertain the cause with certainty j but the specimen said to have that combining weight was of considerable age when analysed.164 THE ANALYST. mate results, is calculated to do very good service in conjunction with the iodine- absorption. As a qualitative test, 1 have found Milliau’s modification of Becchi’s nitrate of silver reaction to be very valuable. It is quite possible that it may be used for obtaining rough quantitative results, but I have not had sufficient experience of it in this direction to express a positive opinion. Milliau’s test certainly seems to be a great improvement on that originally proposed by Becchi, in which rape-oil and amylic alcohol were used with no obvious purpose.My experiments did not indicate that either the melting point or solidifying point of the original sample, or of the fatty acids therefrom, is capable of affording any useful information. The iodine-absorption of a sample of lard-oil was found by Mr. Rowland Williams to be 73 (private communication). A small quantity of lard-oil which I obtained by pressure from lard of known purity showed an iodine-absorption of 74. On the other hand, a sample of lard-oil several years old, believed to be pure, gave only 41, and Muller hae recorded an iodine figure of 47.2. It will be observed that I have determined the iodine-absorptions of the fatty acids of some of the samples, in addition to making the determinations on the original fats.This plan has been recommended by Rose, and Mr. R. Williams has recently recorded some experiments made in the same way. There is one important practical advantage in operating on the fatty acids, and that is that in consequence of their solubility in alcohol, the use of chloroform can be entirely dispensed with. Chloroform is liable to have more or less reducing action on Hubl’s iodine solution, and hence a quantity equal to that used in the test must be employed in the blank experiment for ascertaining the strength of the iodine solution. I f , as sometimes happens, more chloroform has to be added during the analysis to maintain proper solution, an uncer- tainty is introduced, unless another blank experiment be made with a larger quantity of chloroform.All this is avoided if the fatty acids be employed instead of the original fat, and the chloroform wholly omitted. The fatty acids are best prepared by saponi- fying the fat with rectified spirit (not methylated), and the saturated aqueous solution of caustic soda, recommended by Wollny for use in Reichert’s butter process.” A perfectly colourless product is thus obtained. 1 may take this opportunity of cautioning employers of Hubl’s iodine process, of the importance of adhering strickly to the prescribed process, unless the modification adopted be fully described and its effects allowed for. Already there are indications of deviation in detail in manipulation which are liable to cause much trouble and confusion a t a moment when analysts are trying to ascertain within what range the absorptions of lard, cotton-seed oil, and other fats are liable to vary.I have made some experiments with a view of isolating from adulterated lard the fatty acids forming lead salts soluble in ether. The high iodine-absorption of cotton- seed oil being presumably due to the presence of the glyceride of linoleic or similar acid, it would seem to follow that the iodine figure should be higher after the separation of * I have been using Wollny’s modified butter method extensively, and with the most satisfactory results. The improvement in sharpness and certainty amply compensates for the little extra time and trouble involved.THE ANALYST. 165 ~~ _______ the acids of the stearic series. My experiments in this direction have not been very satisfactory, and the tedious nature of the process is such as to discourage one from following up the matter, unless absolutely necessary.I think that the experience we now have shows that cotton-seed oil can be detected with certainty in lard, even when present in very moderate quantity, if it be the sole adulterant. The determination can, at present, only be affected with tolerable accuracy in the absence of beef-stearin. The detection of cotton-seed oil is quite easy, in any case, but the determination becomes more uncertain if beef fat be present. From the combined resnlts of the determinations of iodine-absorption and specific gravity it would be possible to form an idea of the proportion of beef-stearin present in a mixture of that substance with lard and cotton- seed oil. Of course it is necessary to multiply results and to avoid the error of laying down, at this stage, too rigid limits of variation; but the tools we now possess, if used skilfully, appear to be amply sufficient to solve the problem presented to us. I have to thank Mr. W. Chattetway and Mr. W. H. Barraclough for their zealous co-operation and assistance.
ISSN:0003-2654
DOI:10.1039/AN888130161c
出版商:RSC
年代:1888
数据来源: RSC
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On mixed lard and the detection of cotton-seed oil |
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Analyst,
Volume 13,
Issue 9,
1888,
Page 165-167
Otto Hehner,
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摘要:
THE ANALYST. 165 ON MIXED LARD AND THE DETECTION OF COTTON-SEED OIL. BY OTTO HEHNER. (Read at the Meeting, June, 1888.) A BILL has lately been laid before the United States House of Representatives to Regulate the Manufacture and Sale of Counterfeit or Compounded Lard. From the memorial to the Senate and House of Representatives in support of the Bill I take the following interesting details :-- “The annual production of lard in the United States is now estimated at 600,000,000 pounds, of which more than 35 per cent. is an adulteration. Lard is one of the great staple products of the country.” ‘ I The advocates of the proposed legislation do not object to the use of cotton-seed oil as food, either alone or in combination with other substance ; they make no war upon that article.They do not object to the manufacture and sale of any new and healthful article of food ; but they do object to the salt3 of compounds as lard and the concealment of the fact that they are not lard.” the fat of swine after being melted and separated frorr. the flesh,” ‘ I not any particular part of the fat, but whatever is the fat of swine thus treated is lard; that is the generic name.” I n 1886-7, 17 million hogs went to market, the lard from which alone amounted to more than 527 million pounds, representing a value of 40 million dollars. More than 325 million of pounds of it were exported to foreign markets, bringing into the United States nearly or quite 30 million dollars.” ‘‘ Forty years ago reJined lard came largely into use. It was made by pressing out of pure lard a portion of the oil, the lard stearine being left behind.This was added to unpressed lard for the purpose of stiffening it, the mixture being called reJined Znrd, consisting entirely of the fat of swine. It commanded for 40 years a higher price They define lard as166 THE ANALYST. than ordinary lard, the differewe being on the average one half cent in favour of the refined article.” “ During the last seven or eight years compounds have been made consisting of lard, cotton-seed oil, and beef stearinel; or lard, water, cotton-seed oil, and beef stearine ; or cotton-seed oil, beef stearine, and no lard, or only a very faint trace of lard. These compounds were sold as ‘ refined lard,’ ‘ pure refined lard,’ ‘ choice refined family lard,’ and other similar names.” Professor H.W. Wiley, in his evidence, states that “ he analysed 13 samples of Fair- bank’s manufacture, all of which contained cotton-seed oil, eight being branded ‘ Prime refined family lard,’ one ‘ Choice refined family lard,’ one ‘ Pure refined family lard,’ one ‘ Prime refined family lard,’ and one only ‘ Compound lard.’ Of 12 samples of Armour and Co.’s manufacture ten contained cotton-seed oil, two being pure lard.” 6‘ Messrs. Armour and Co. state that they use from 59 to 75 per cent. of lard i n their mixtures, Fairbank from 50 to 75 per cent. The former firm use 75,000 barrels of cotton-seed oil, and make 60 million pounds refined lard. 75,000 barrels weigh 28,125,000 pounds ; hence the average proportion would be 46 per cent. of cotton-seed oil in the mixture.But as from 10 to 15 per cent. of stearine are necessary to stiffen the mixture, the proportion of lard would be only about 42 per cent.” Abundant evidence was collected in proof of the above statements, but I would take exception to the statement that lard is the fat of swine generally. Of late years certainly the whole of the fat has been used in the manufacture of lard, but originally only the belly fat was employed. The test relied upon by Professor Wiley for the detection of cotton-seed oil is the nitrate of silver test, presumably that described by E. Bechi. This has, since its publi- cation in 1884, been variously modified. Bechi dissolves 1 grain of silver nitrate in 200 C.C. of 98 per cent. alcohol, and adds 40 C.C. ether.He also makes a solution of 15 per cent, of rape oil in alcohol. 10 C.C. of the oil to be examined are mixed in a flask with 1 C.C. of the silver solution, and 13 C.C. of the alcoholic rape oil solution ; the whole is well shaken and heated for a quarter to half an hour upon the water bath. In presence of cotton oil the mixture assumes a dark colouration. The Italian aovernment at once appointed a commission t o investigate the method. The re- port is to the effect that the method is perfectly trustworthy, provided the reagent contains a small quantity of pure nitric acid, and the oils to be tested have previously been filtered. This is the true source of lard. The reagents recommended are composed as follows :- 1. Silver nitrate, 1 grm. Alcohol, 200 grms, Ether 40 99 Nitric acid, *1 grm, 2.Amylic alcohol, 100 grms. Colza oil 15 9 , Pifteen per cent. of cotton oil can readily be detected in olive oil, but if less than 10 per cent. ore present the results are doubtful. I f too little free acid bo present, reduction may take place even in absence of ootton oil; if too much, no reduction takes place even with cotton oil.THE ANALYST. 167 Milliau (ANALYST, xiii., p. 95), instead of testing the oils direct, separates the fatty acids, takes about 5 C.C. and heats with 2 C.C. of a 30 per cent. aqueous solution of nitrate of silver. In this manner he claims to have easily detected a one per cent. adulteration. I have made many experiments with pure and mixed lards, and can fully corroborate the Italian Commission as to the importanco of the presence of a small quantity of free nitric acid, but Bechi's test can, without impairment of its delicacy, be simplified by the omission of the amylic solution of colza oil.I make a solution of nitrate of silver in alcohol and ether, very slightly acidified, and add to the oil to be examined about half of its bulk of the silver solution, then heat on the water bath for a quarter of an hour, no longer. Pure lard always remains perfectly unchanged, cotton oil mixtures blacken more or less quickly. It is quite possible to arrive at approximately quantitative results, by comparing the oil mixtures of known composition. I consider the test an invaluable one. Pure butter does not reduce the silver solution ; margarine, containing as it does almost in- variably some cotton oil, reduces strongly. I can see no advantage in Milliau's modi- fication, especially as it renders the test a much more complicated one.As to the quantitative estimation of cotton oil in lard, the Maumh6 reaction, if properly applied, answers all requirements. It is ersential that the sample to be tested be free from water. If the lard does not melt quite clear, it must be heated over a very small naked flame, until all water is driven off. Fifty grammes of pure lard with 10 C.C. of strong snlphuric acid show ti rise of from 24 to 27.5 degrees Centigrade, cotton oil of about 70 degs. Mixtures made by myself yielded increase of temperature a4 nearly as possible corresponding t o the theory. I n every case a lard which reduces silver shows a rise higher than 27.5 dega.Thus I have examined samples which produce tt rise of 29, 35, 36, 38.5, 40, and 41.5 degs., the first sample reducing silver slightly but unmistakably. If in any doubtful case further corroboration is required, the method lately described by E. Salkowski (Zecht. Anal. Clzem. xxvi., 557) is extremely useful. Salkowski has shown that, whilst animal fats contain invariably a small quantity of cholesterin, vegetable fats contain an allied substance, phytosterin. The former crystallises from alcohol in flat tablets, melting at 1 4 6 O ; the latter in long needles, fusing at 132" C. It is very easy to obtain a tangible quantity of the crystals from 50 grammes of the fat. This is saponified with alcoholic potash, the soap well shaken out with ether, the ether distilled off, the residue once more treated with alcoholic potash and ether, and the residue thus purified dissolved on a watch-glass in a few drops of hot alcohol. The long needles of phytosterin obtained in the case of the presence of a vegetable fat can be further tested by the reaction with chloroform and sulphuric acid. Cholesterin gives a beautiful red chloroform solution, phytosterin a bluish one, the difference being strongly marked if the solution is allowed to stand, in a well-corked test-tube, for a couple of days. I rely, therefore, upon the silver test, coupled with MaumBnB's method, and car- roborate, if requisite, by that of Salkowski. It is also quite applicable to butter and margarine.
ISSN:0003-2654
DOI:10.1039/AN8881300165
出版商:RSC
年代:1888
数据来源: RSC
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“On the adulteration of lard with cotton-seed oil” |
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Analyst,
Volume 13,
Issue 9,
1888,
Page 168-169
Rowland Williams,
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摘要:
168 THE ANALYST. “ON THE ADULTERATION OF LARD WITH COTTON-SEED OIL.” BY ROWLAND WILLIAMS, F.T.C., F.C.S. (Bead at the Meeting, June, 1888.) DURING the past few months I have had very extensive experience in connection with lard adulteration. O u r worthy President, having become aware of the fact, suggested that I should write a short paper, supplementary to the note on the same subject which he himself has read this evening. It gives me great pleasure to fall in with Mr. Allen’s suggestion, and I can only express my regret that my remarks must of necessity be very brief. I should have liked to go into the matter much more exhaustively, but time forbids. Saponijcation, equivalent.-Koettstorfer’s process is quite useless, so far as the detec- tion of cotton-seed oil in lard is concerned, as both require practically the same amount of alkali for saponification. This fact will, no doubt, already be so well known to those among you who are regularly engaged in food analysis, that it is, perhaps, almost super- fluous to mention it.Determination of the saponification equivalent of lard is, however, occasionally useful, as any great deviation from the normal figure would indicate the presence of some adulterant-cocoanut oil, for instance, which is said to be sometimes used for sophisticating lard. Xelting Point.-The melting point of lard is no criterion as to its freedom from adulteration, as the question of a high or low melting point depends entirely upon the part or parts from which the fat is obtained. X;ciec;Ji~ Gmwity.-Inasmuch a3 the specific gravity of pure lard a t 212” Fah.is about -8G1, while that of cotton-seed a t the same temperature is about *872, it seemed possible that the presence or absence of cotton-seed oil might be ascertained by a careful deter- mination of the density of the sample at the temperature of boiling water. I have found that a large proportion of cotton-seed oil does undoubtedly raise the specific gravity of lard t o a moderate extent, but a small percentage affects the result very slightly, so that, according to my experience, no very definite information can be obtained by these means. HaurnenZ’s Test.-As cotton-seed oil gives a very considerable rise of temperature when treated with strong sulphuric acid, while pure lard gives only a moderate increase, I applied Maurnend’s test to several suspected samples with a view to ascertain whether cotton-seed oil could be detected in that way, but for some reason or other I did not obtaih satisfactory results.Even with samples which undoubtedly contained large pro- portions of the adulterant, Maumenk’s test has in my hands failed to determine anything like the real extent of sophistication, I understand, however, that a London chemist has found this method to answer fairly well in the case of lards heavily adulterated with cotton-seed oil, but for my own part I consider Maumenb’s test too dependent upon mode of manipulation and various other circumstances to yield really reliable infor- mation, Iodine Absorption.-This is the tost upon which I chiefly rely for the determination of cotton-seed oil in lard, in the absence of interfering bodies.By the latter I more particularly refer t o stearin, which is sometimes added in rather large proportion to lard which has been adulterated with cotton-seed oil, in order to neutralise the softeningTHE ANALYST. 169 effect produced by the latter. As stearin absorbs only about one-third as much iodine as cotton-seed oil, the addition of a large percentage of the former naturally reduces the iodine absorption of the mixture to a greater or less extent. Still, I have rarely found the stearin to interfere sufficiently t o absolutely nullify the iodine absorption test. Out of the numerous samples of lard submitted to me for analysis, all of those which I believe to be genuine (with one exception) absorbed from 60 to 62 per cent.iodine. Most of these lards, I may say, were of American origin. English lard is said to have a somewhat lower iodine absorption, but I cannot speak with certainty on this point. The peculiar sample just referred to, and said to be leaf lard, absorbed only 51 per cent, iodine-a result for which I am unable t o offer any satisfactory explanation. Mr, Allen informs me, however, that a sample of lard prepared from the omentum, which he has just examined, had an iodine absorption of 55.4 per cent. I myself have to-day rendered some lard from the leaf, and this, I find, absorbs 51.8 per cent. iodine. Allen’s Organic Analysis ” (Vol. II., page 50) it will be found that Hiibl himself (who may be regarded as the originator of this test) gives the iodine absorption of lard as 59 per cent., whilst other observers give it as 61 per cent., figures so close to my own as to render the probability of 60 per cent.or thereabouts being the true iodine absorption of ordinary lard, made from the fat of the entire animal. I have found samples of refined cotton-seed oil and beef stearin-such as are used for the purpose of adulterating lard--to absorb respec- tively 110 and 21 per cent. iodine. Some of the lards which I have examined absorbed as much as 85 per cent. iodine, and I frequently meet with samples having iodine absorptions of 70 to 75 per cent. There can be no doubt whatever about samples such as these being largely adulterated with cotton-seed oil. It should be mentioned that lard dealers can detect even small proportions of cotton-seed oil by the taste and smell, but it has only recently become possible to prove the fraud by scientific evidence.Silver Nitrate Test.--Milliau’s modification of Bechi’s original process for detecting cotton-seed oil in olive oil has so recently been described in THE ANALYST (May 1888, page 95) that it is unnecessary for me to give the modus opeyandi. I have applied the test to a large number of samples of lard, and find it to answer exceedingly well for the detection of cotton-seed oil. I have examined the fatty acids from numerous other oils and fats, all of which have been free from reducing action on silver nitrate. The reaction seems, therefore, characteristic of cotton-seed oil. It is advisable to make a blank experiment with the reagents, as I find even ‘‘ pure” alcohol occasionally contains impurities which reduce silver nitrate to some extent. The silver nitrate test, although undoubtedly of great value as a means of detecting cotton- seed oil in lard, etc, has, I believe, hitherto been used only qualitatively. When employed in the ordinary way it simply indicates the presence or absence of cotton-seed oil, without giving much, if any, idea of the percentage present. During the last few days I have been engaged on a series of experiments with a view to make the process quantitative. So far, however, I have not been successful, but if further experiments prove more satisfactory, I shall be pleased to bring my results before you upon some future occasion. 1 should like t o call your attention to the fact that in
ISSN:0003-2654
DOI:10.1039/AN8881300168
出版商:RSC
年代:1888
数据来源: RSC
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Lard adulterated with cotton-seed oil |
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Analyst,
Volume 13,
Issue 9,
1888,
Page 170-171
E. W. T. Jones,
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摘要:
-- 170 THE ANALYST. ---, LARD ADULTERATED WITH COTTON-SEED OIL. BY E. W. T. JONES, W.1.C. (Read at the Meeting, June, 1888.) I BELIEVE I was the first public analyst to officially certify under the Sale of Food and Drugs Act this adulteration ; hence a few words from me as to the means I rely on for detecting and estimating it may be acceptable to those analysts who may not have yet given the matter their special attention. I do not claim any originality for the reactions involved, but simply point out their application. The first test I apply is a qualitative one, based on the well-known action of S,CI, on certain oils. With lard I proceed as follows :-5 grms., which when melted may be pipetted with a tube made to deliver this weight, are put into a small porcelain dish, and just before setting, 2 C.C.of a mixture of equal volumes of S,CI, and CS, carefully pipetted into it, and the mixture well stirred a t first, and then occasionally for the first quarter of an hour or so. Do not apply heat, but simply allow to stand on the labora- tory table ; by this treatment genuine lard only thickens, or perhaps becomes rather stif7 in three hours ; but if it contains any real amount of cotton-seed oil, it becomes quite hard ac?ad solid in half this time. This test is very simple, but, with practice, one can with a certainty pick out all lards containing cotton-seed oil. For estimating the adulteration I rely on the I absorption from Hubl’s reagent, made by dissolving 5 grms. I in 100 C.C. of 95 per cent. alcohol and 6 grms. HgCI, in 100 C.C. of such alcohol, then mixing and allowing to stand at least over night before use.I drop 20 to 22 drops of the melted lard into a weighed 3-oz. wide-mouth stoppered bottle, and carefully re-weigh, the weight of fat not to sensibly exceed 0.5 grm. ; just melt by putting the bottle for a minuto or so on the top of the water oven, and when nearly cool again, add 10 c (1. of pnre CHC‘I,, and so dissolve the fat. When quite cold, add 20 C.C. of the Hub1 reagent, very carefully measured, and allow to stand three hours; the colour must, then he decidedly brown, showing excess of I, or else less fat miist be taken for the quantity of Hiibl reagent. I object to the addition of more Hub1 after the experiment shows too little I, but prefer to commence again with less fat.After standing the prescribed time, the contents of the bottle are transferred to a beakor, the bottle rinsed with KI solution, of which enough must be added to dissolve the I, and the solution then diluted to 150 to 300 c.c., and the frco I estimated with ‘‘ Hypo ” solution and starch; the amount of I now found being taken from what the 20 C.C. Hub1 contained leaves the amount absorbed by the quantity of fat employed, and is to be calculated to a percentage. I standardize the ‘(Hypo” just ?)gore use with fiome pure I, carefully weighed (about 0.5 grm.), and SO find its exact factor. I take the “ Hypo ” equivalent of the 20 C.C. Hubl with each set of experiments. Example with pure Lard. Fat taken, 0.5660 grm. + 20 C.C. Hubl, after 3 hours took 9.4 C.C. ;‘ Hypo.” 20 C.C.Hubl took 35.6 C.C. (‘ Hypo,” -5005 grm. I took 39.2 c.c, (‘ Hypo,” hence 5005 - 39.2 = *0127678 I for 1 C.C. (Log 2*1061180)THE ANALYST. 171 Using logarithms makes the calculation very easy and exact. I find genuine lard never takes sensibly more than 60 per cent, I, whilst cotton- I adopt the formula- seed oil takes from 105 to 110 per cent. 100 (=be=') 45 = per cent. cotton-seed oil. To support the foregoing tests I also take the Sp. Gr. of the lard (ZJ looo Fahr. I find the Sp. Gr. of pure lard under such circumstances to be 906.0, and of cotton-seed oil 9 13.5, hence- ("". Gr. f7q;d - 906) = per cent. cotton-seed oil. Genuine Commercial Lard. Sp. Gr. at looo Fahr. Not taken 906.; . . 906.4 . . 906-0 . . 905.8 . . 906.1 , . 906.1 . . 905.7 . . 906.0 , . . . .. . . .. . . . . .. .. . . . . . . .. . . .. .. .. * . " . . . . . I per cent. * . 59.90 .. 59.10 .. 56.47 .. 56.56 .. 59.04 .. 57.39 .. 59-90 .. 60.42 . . 69.50 . . 61-31 - Average. .906.0 . . .. . . . . 58.9 TABLE SHOWING R,ESVLTS CALCULATED FROM THE SP. GR, AND THE I. Cotton-seed oil Cotton-seed oil Sp. Gr. at calculated by IQ calculated by 100" Fahr. sp. Gr. fd. - 906 ( Mixture made of f 908.5 908.7 908.4 907.4 906.9 907.5 907.3 907.9 907.4 907.7 907.3 907.2 906.9 2 parts lard andJ' seed oil. \ 1 part cotton- 33 36 32 18 12 20 17 25 19 23 18 17 13 74.25 76.53 75.26 67.22 65-3 67.3 67-8 69.3 66.7 68.5 68-63 67.7 65-65 32 36 34 16 12 16 17 21 15 i 9 19 17 13
ISSN:0003-2654
DOI:10.1039/AN8881300170
出版商:RSC
年代:1888
数据来源: RSC
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5. |
Detection and estimation of cotton-seed oil in lard |
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Analyst,
Volume 13,
Issue 9,
1888,
Page 172-174
W. F. K. Stock,
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摘要:
172 THE ANALYST. ~ DETECTION AND ESTIMATION OF COTTON-SEED OIL I N LARD. BY W. F. K. STOCK, F.C.S., F.I.C. THE method about to be described is a modification of that devised by Milliau, of which an abstract appears in the ANALYST (vol. xiii., p. 95). AS there described, Milliau’s process has failed, in the hands of the present writer, to give satisfactory results; but he does not ascribe the irregularities observed to anything but want of detail; for which, probably, Milliau is in no way to blame, since the article in the ANALYST is not an original communication. As worked in the present writer’s laboratory the process stands as follows :- 15 grms. of the sample are saponified in a 7-inch porcelain basin with a mixture of 15 C.S. of 30 per cent, NaHO, and 15 C.C. of 92 per cent.alcohol. To commence, the fat is heated to 110W. The alkaline alcohol must be added in quantities not exceeding 1 C.C. at a time, the temperature not being allowed to fall below 95OC. to 100°C., constant stirring at this part of the operation being most important. If the saponification has been successful, the resultant soap is a smooth thick paste. Boiling distilled water is now added drop by drop, a thin flexible spatula being used to break down the paste. When this has the appearance of smooth starch, water may be run in till a volume of 500 C.C. is reached. 40 C.C. of diluted sulphuric acid (1 -10) are now added to the contents of the basin, the liquid is stirred gently and brought to boil for 7 to 12 minutes, then kept just below boiling, until the separated fatty acids fuse to a clear oily layer.The greater bulk of the acid watery liquid is siphoned off, the remainder, with the fatty acids being poured into a clean warm flask with a somewhat long and narrow neck. The fatty acids are freed as nearly as possible by siphonage from the watery under layer, and the flask is filled up with boiling water so as to bring the fatty acids into the neck, by which operation a partial washing is given, 5 C.C. of the fused fatty acids are now transferred by means of a dry, warm, fast-running pipette, into a clean, dry, wide test tube. 20 C.C. of abaolute alcohol are added: care being taken to wash the pipette by running the alcohol through it. The contents of the test tube are heated to incipient ebullition in a vessel of boiling water. 2 C.C.of a 30 per cent. solution of silver nitrate are now rapidly poured into the tube, when if even 2 per cent. of cotton-seed oil be present in the sample the characteristic cedar-brown colour is at once developed. Pure lard gives absolutely no colour. To quantify this reaction, known mixtures of pure lard and refined cotton-seed oil are treated exactly as above, and the colours in the different tubes compared by reflected light against a white background. This must be done simultaneously, for in about seven minutes the colouring matter begins to fall out, and correct comparison is then impossible, Complete solution should follow. In careful hands excellent results are obtainable. DISCUSSION. Mr. HEHNER read the following letter from Prof. J.Campbell Brown :- DEAR SIR,-AS I cannot attend the meeting of Public Analysts’ Society to- morrow, I am anxious that if the paper doea not deal with the following points, you University College, Liverpool, June 19th, 1888.THE ANALYST. 173 should call the attention of the meeting for me to the two errors analysts are liable to make if they trust to the iodine equivalents already published. 1. They are liable to greatly under-estimate the proportion of cotton-seed oil and other foreign fats in adulterated lard. The substance used by about twenty-five of the American firms is a mixture of cotton-seed oil and beef-stearin, the residue from the manufacturer of oleo-margarine. Now, while the iodine equivalent is high, 105 to 110, the iodine equivalent of commercial stearin is low, under 30.And the iodine equiva- lent of any mixture that can be used for mixing in large proportions with lard is much lower than that of cotton-seed oil-not higher, if so high, as between SO and 90. Now if any one calculates the quantity of cotton-seed oil in mixed lard giving an iodine equivalent of say 76, using 105 as the iodine equivalent of the foreign fat, instead of 90 or under, it is:clear that he will greatly under-estimate the quantity of foreign fat. He will even under-estimate the cotton-seed oil portion of the foreign fat. 2. They are liable, on the other hand, to condemn genuine lakd which is more oily thanpork fat or lard rendered in this country. American lard contains as a rule naturally much more olein than our own. If some of the lard oil has not been pressed out, the high iodine equivalent of lard oil- from 75 to SO-SO raises the one equivalent of the thin oily lard, that an analyst judg- ing mainly from the iodine equivalent would infer the presence of cotton-seed oil where there was only excess of lard oil.It is necessary, therefore, to be very careful in deter- mining, first the presence of some cotton-seed oil by safe qualitative tests before deter- mining the iodine equivalent ; and it is further necessary, in order to avoid both the errors I have mentioned, to take into consideration the consistency of the sample, and attend to tests for beef-stearin, in drawing any conclusion from its iodine equivalent. Kindly bring these points before the meeting as from me, unless they are fully gone into in the paper.--l am, yours truly, The Secretary, Society of Public Analysts.Mr. HARLAND said that the American manufacturers’ plan was t o express the lard oil from the lard and replace it by cotton-seed oil. Working on these lines in the laboratory, he had found that about ten per cent. of lard oil can be squeezed out of genuine lards, but that adulterated samples of various American manufacturers gave thirty, forty, or fifty per cant. of what appeared t o be, by its sp. gr. and solidifying point, cotton-seed oil. Mr. WATSON GREY gave the following figures for the percentage of iodine absorbed by various kinds of lard when treated by Hubl’s process :- J. CAMPBELL BROWN. Iodine Kind of lard. absorption. From omentum of hog ..............................49.5 Market lard (bought in Liverpool) ............... 49 From omentum of sow .............................. 55.5 From back of pig .................................... 65 He would fix the average at 57. If this was accepted, it would account for the fact that the President, having taken 62 as the standard number, had found that, whereas the sp. gr. of one adulterated sample corresponded t o thirty per cent. of cotton-seed oil, the iodine absorption indicated only fifteen per cent., without having recourse to the suppo- sition that tkllow was present as well as cotton-seed oil. His experience went to show that the silver nitrate test-at least, in its unmodified form (without the addition of free nitric acid)-was rather unsatisfactory. Mr. Fox stated that he had recently found fifky per cent. of earth-nut oil in lard oil, detecting it by the altered ~ p . gr. and the presence of arachidic acid.174 THE ANALYST. ~~ ~ ~ ~ ~~ ~ ~ Mr. JONES, in reply to a remark of the President's on his practice of taking the sp. gr. of fats at 100" F., admitted that it was rather an old-faqhioned plan, and con- templated changing it. He had not found it necessary to use concentrated aqueous caustic alkali and fresh alcohol when saponifying oils in order to get white fatty acids, as proposed by the President, the alcohol he obtained in Wolverhampton not turning brown from the action of caustic alkali, even when kept for several months.
ISSN:0003-2654
DOI:10.1039/AN8881300172
出版商:RSC
年代:1888
数据来源: RSC
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6. |
“Water reports—a dilemma.” |
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Analyst,
Volume 13,
Issue 9,
1888,
Page 174-176
Matthew Adams,
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摘要:
174 THE ANALYST. “ WATER REPORTS-A DILEMMA.” BY DR. MATTHEW ADAMS. (Read at Meeting, July, 1888.) THE subject of “Polluted Drinking Water and the Closure of Wells,” brought forward for discussion by Dr. Hill at the June meeting of our Society, is of sufficient importance to warrant my placing before you a correspondence which passed between me and the Urban Sanitary Authority of Rochester. This correspondence shows a position of affairs the very reverse of that which Dr. Hill found himself placed in. He fell upon the legal horn ; I was impaled by an equally tormenting official horn. I n such a dilemma what can be done? WATER ANALYSIS.-REPORT. To Richard Prall, Esq., Town Clerk. Total Solid Matter ............ Loss on Ignition., ............ Chlorine .................... Nitrogen;as Nitrates and Nitrites Phosphoric Acid.............. 5 (Free Ammonia .............. j Albuminoid Ammonia . . . . . . . . 5 1 Oxygen absorbed in 4 hours . . . . Appearance in 2-foot tube. . . . . . .% I Oxygen absorbed in 15 minutes 0 Total Hardness (Clark‘s Scale). . Permanent hardness after boiling I 77.3 5.1 7.7 1-14 -02 -05 -025 -044 27-5 12.0 gr. blue 57.1 3.4 5.4 1.14 -00 604 -005 -056 24.0 11.1 p. blue sus. mat. 71.4 4.6 7.0 1.43 *OO *02 ,028 -036 2 6.0 13.5 pale cl. blue Slight 46.6 2.2 4.3 *95 .oo .02 *013 -028 iowo 9.0 pale el. blue None - @p All results are given in Grains per gallon, except Free and Albuminoid Ammonia, which are in Darts Der million. OBSERVATIONS. SIR, 31st May, 1883. Herewith I hand you results of my analyses of fobr samples of water recently received from you for analysis, from all of which data I judge that Nos.1,2, and S-especially Nos. 1 and Cour,ty and Borough Analyst’s Laboratories, Ashford Road, Maidstone.THE ANALYST. 175 - 2-are more or less tainted, and my advice is they should not be used for drinking purposes i€ better is a t hand. At the same time I am bound t o say there is not much indication of ACTIVELY dangerous pollution. The polluting matter is for the most part oxidized and so rendered inert, but this oxidation is not t o be always relied upon, therefore such waters must be considered treacherous and dangerous. I am, Sir, Yours obediently, MATTHEW A. ADAMS. Local Government Board, Whitehall, 8. W. September 4th, 1883. Sm, I am directed by the Local Government Board to advert t o your letter of the 8th ult., stating with reference to certain wells in the town of Rochester, that the U.S.A.do not consider that they could obtain orders to compel the closing of such wells. The Board direct me to state that having regard to the fact that the wells in question derive their supply from a soil which is miich befouled by cesspools in near proximity to them, they are of opinion that measures should a t once be taken by the S.A. to secure their closure, an opinion which appears to the Board to be fully borne out by the statements of the Analyst to whom thelwaters were submitted. I am, however, to point out that, quite apart from the positive evidence as to pollution which chemical analysis has in this case afforded, the Board in forming an opinion as to the wholesomeness or not of a water have regard rather to a full knowledge of its sources and of the local conditions by which it is liable to be affected than to its mere chemical ingredients.I n this conection I am t o direct the attention of the Sanitary Authority t o pages xvii. t o xxi. of the accompanying print of the recent report of their medical officer with especial reference t o the opinion expressed on page xxi., ‘I that we must go beyond the laboratory for evidence of any drinking water being free from dangerous organic pollution.” I am further t o state that the expressions used by the Analyst, and especially with reference to the polluting matter being ‘ I for the most part oxidized,” appear to show an inadequate view of the conditions under which water can safely be used.In the present case it appears to the Board that if the Authority are still of opinion that their action might be hindered by some qualifications expressed by the Analyst they should procure fresh analyses of the waters by some well-known chemist, and if necessary the analysis should be repeated until any varying qualities of the several well waters have been fully ascertained, and conclusive inference has been drawn respecting the risk to these sources of With regard to the soaka e from cesspools, the Board would call the attention of the Sanitary Authority to their powers unfer Section 47 (3) of the Public Health Act, 1876, but they think i t proper to add in this connection that to prevent for the future the contents of a privy or cesspool to soak therefrom will not render wholesome the water derived from a soil into which such contents have already soaked in notable quantity.I am to add that under Section 62 of the Act, the Sanitary Authority might compel the Brompton, etc., Waterworks Co.’s water to be laid on in any case where it appears on the report of the Surveyor that any house within the district is without a prcper supply of water, and that such a supply of water can be furnished thereto a t a cost not exceeding the water rate anthorised by the Local Act in force within the district. SUPPlY. 1 am, Sir, your obedient servant, ALFRED D. ADRIAN, Assistant Xecretary. a To Richard Prall, Esq., Town Clerk, Rochester. September loth, 1883. D ~ A R SIR, Having regard to my report of May 31st on these four samples of water, and the letter from the Local Government Board of the 4th inst., I have to remark: that it is not for me as your chemical adviser “to go beyond the laboratory.” It is my duty to form an independent opinion derived from chemical data alone ; others, such as your Medical Officer of Health and Inspector of Nuisances, must advise you as t o local surrounding circumstances ; moreover, you have a right to expect practical and not theoretioal advice, such as may reasonably be expected,176 THE ANALYST.successfully to stand the test of opposition in court ; all this you have a.nd no one having respect for his chemical reputation could say more than I have done, via., that Nos, 1, 2, and 3 are treacherous and dangerous, and should not be used for drinking purposes.I am, dear Sir, Yours obediently, MATTHEW A. ADAMS. x- To Richard Prall, Esq., Town Clerk, Rochester. September loth, 1883. DEAR SIR, I beg to return Local Government Board’s letter ’and printed report tf their Medical Officer, together with my remarks thereon. With regard t o the ‘‘ expressions in my original report referred to in that letter, t o the effect that the polluting matter, being “ for the most part oxidized,” showed (on my part) an inadequate view ;of the conditions under which water can be safely used, I have simply to say that to the best of my belief, Dr. Dupre, the Local Government Board’s own analyst, would endorse every figure and word I have used, and to my mind i t would be an undoubted proof of inadequacy and incompetency to lead your authority t o overlook the all-important distinction between oxidised and unoxidised organic matter. Their suggestion that the analyses should be repeated until any varying qualities of the several waters have been fully ascertained, etc., is a good one, If on repeated analyses, changes in the constituent parts can be shown to occur, that together with the evidence already attained-would put the case in a much stronger light as against the wholesomeness of the waters. But there is no occasion for this, especially after the Local Government Board’s letter ; the water ought to be condemned, and if it is necessary I will come over and support this advice in the witness-box. Yours faithfully, MATTHEW A. ADAMS. (Conclusion of the Society’s Proceedings.)
ISSN:0003-2654
DOI:10.1039/AN8881300174
出版商:RSC
年代:1888
数据来源: RSC
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7. |
Estimation of glycerin in the crude article |
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Analyst,
Volume 13,
Issue 9,
1888,
Page 176-178
R. Benedikt,
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摘要:
176 THE ANALYST. ESTIMATION OF GLYCERIN I N THE CRUDE ARTICLE. R. BENEDIKT AND M. CANTOR.* POR the determination of the commercial value of crude glycerins, there does not as yet exist an easy and trustworthy process. Most of the processes as yet proposed give uncertain results, particularly the one based on the oxidation with chromic acid, as many other organic bodies are also oxidised to carbonic anhydride and water. The process with permanganate by Benedikt and Zsigmondy has certainly given good results, but in the case of crude glycerin the sample must first be diluted, then treated with subacetate of lead, and the excess of the latter be removed by sulphuric acid before we can titrate. It. Diez has applied Baumann’s test for the estimation of glycerin in wines, etc. The solution is agitated with soda ley and benzoil chloride.The precipitate, consisting of glycerin di and tribenzoate, is weighed, an allowance being made for solubility. Although we will not dispute the use of this process when applied to wine analysis, me have never suc- ceeded in getting correct results with it in the case of crude glycerins, even by scrupulously following Diez’s directions. The error amounted from 3 to 8 per cent. of the total glycerin. We now propose the Acetin process, which gives quick and correct results, and is based on the following principle. Glycerin on boiling with acetic anhydride passes completely into triacetin. If water now be added, and the amount of uncombined acid exactly neutralised with soda, the combined acid may be easily ascertained by saponifying with excess of soda, and titrating back with standard acid.* Zeitschr. f. angew Chemie, A?. 16. The following solutions are required :-THE ANALYST. 177 1. Half normal or normal hydrochloric acid, the exact strength of which must be 2. A solution of 20 grammes of sodic hydrate in a litre of water, 3. 10 per cent. caustic soda in a flask holding about 1% litro. ascertained with the greatest care. The flask is closed by an india-rubber cork, through which passes a 25 C.C. pipette, the top of which is closed by an india-rubber tube, and a clamp. About 1.6 grm. of the sample is weighed in a wide-neck flask with round bottom; 7 grammes of acetic anhydride and 3 grammes of anhydrous sodic acetate are added, and the whole boiled foi one and a half hours under an upright condenser.After it has somewhat cooled, 50 C.C. of water are added, and the mixture once more brought up to the boiling point. This must also be done under upright condenser, asthe triacetin is sensibly volatile in water vapour. After the oily mass has dissolved, the liquid is filtered into a wide-necked flask of about 600 C.C. capacity. A white flocculent precipitate, which is rather large in crude glycerins, remains in the filter, and must be well washed. After complete cooling, phenol-phthalein is added, and the fluid j u s t neutralised with No. 2 sodic hydrate. The point of neutrality is reached when the fluid turns yellowish-red. Care must be taken that in doing the check, the pipette shall deliver exactly the same quantity.After boiling for a quarter of an hour, the excess of alkali is titrated back with the acid No. 1. The pipette (No. 3) is now filled, and the contents delivered into the flask. EXAMPLE, 25 C.C. alkali , . .. .. .. . . = 60.5 C.C. N acid. Titrated back with . . .. .. . . 21.5 ,, 9 9 Triacetin is equivalent to 39.0 ,, 9 , Taken 1.324 grammes of glycerin. -- 1 c,c. of acid representing *03067 grm. of glycerin, the sample contains 90.3 per cent. Testing fats for diglycerides: from the ease with which glycerin can be made into triacetin, we may conclude that the mono or diglycerides of the higher fatty acids may be readily converted into triacetin by boiling with acetic anhydride. Another aid to the accurate analysis of fats is thereby obtained, as it is easy to directly estimate the per centage of mono or diglyceride a sample may contain.Let M be the molecular weights of the diglyceride, a the saponification number of the fat before, and b after the acetyling, then as 56 stands for KHO, and 42 for the residue C,H,O, the percentage of diglyceride will be- 100 M ( b - a ) 5600-42 b. For instance, the stearin from colza oil has to be examined for dierucin C,H,(OC,,H*,),OH. We first determine the saponification equivalent, then acetyylise 90 to 60. grammes of fat, according to the directions of Benedikt and Ulzer, and estimate the saponification178 THE ANALYST. number again. molecular weight is 732. If a = 46, and b = 674, then D = cent. dierucin. If the amount of diglycerides is very small, the combined acetic acid is better esti- mated by Reichert’s process, The calculation is somewhat more troublesome if the fat contains glycerides of oxyztcids, as these give also an acetyl number.I n this case we isolate the fatty acids first, and then determine their acetyl equivalent. Reimer and Will particularly point out that colza oil contains an oleic acid, which is isomeric with the oleic acid of castor oil. This is, however, contradicted by its low acetyl number, which they found to be 6.3, corresponding with 3.8 per cent. oxyoleic acids. The true composition of colza oil is not as yet known with certainty, then its 100, whilst the acids which Reimer and Will have isolated give a far lower figure: erucic acid 75.2, benic acid = 0, rapinic acid 85-2. It is, therefore, probable that a large proportion of another acid of the linseed oiI type must be present. Dierucin is the only glyceride as yet isolated from naturalfats, but it must yet be ascertained if it really exists in the fresh oil. Allen has lately suggested that Japan wax contains dipalmitin. The direct test gave a negative result. The saponification equivalents of the original and acetylised wax were found to be the same, viz., 222. On saponifying butter with an .insufficiency of alcoholic potash, Bell got an oily substance, melting at 4*4OC. We have repeated this experiment, and indeed obtained a thinnish %oil, with a strong butyric ether smell, which, however, did not yield any glycerin, and must therefore have consisted for the greater part of ethylic ethers. For pure dierucin this is 153.3, for acetylised dierucin 217.4. The 100 x 732 x 21.8 = 3o per 5600 - 42 x 67.8 dine absorption power
ISSN:0003-2654
DOI:10.1039/AN8881300176
出版商:RSC
年代:1888
数据来源: RSC
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8. |
Monthly record of general researches in Analytical Chemistry |
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Analyst,
Volume 13,
Issue 9,
1888,
Page 178-179
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摘要:
178 THE ANALYST. MONTHLY RECORD OF GENERAL RESEAECHES I N ANALYTICAL CHEMISTRY. BY THE FILTER. L~J. DE KONINCK. Zeitschr f. anal Chemie, A'o. 15.-About twelve years ago, a method for the estimation of potash was recommended by Fresenius, whereby the use of the weighed filter was avoided. The platinum precipitate was col- lected on a filter, and after drying, the bulk of it was carefully removed. The minute quantity still adhering was now removed by treatment with boiling water, and this solution evaporated in a weighed dish. After adding the chief precipitate, the whole was dried and then weighed. The author has extended the idea to a number of other metals. A ~ ~ o u r u ~ ~ - - T h s platinic ammonium precipitate may be treated like the potassium compound. ARsENIc.--The triple arsedate ia carefully removed from the filter and put info ft crucible. The filter is repeatedly washed *ith small quantitie8 of dilute nitric acid, and the liquid is evaporated to dryness in the same crucible.When completely dry the whole is gradually heated to redness, when a pure magneeic pyro-arseniate is formed without the least loss of arsenic, AVOIDING TIIE USE OF WEIGHED FILTERS AND THE REDUCTION OF PRECIPITATESTHE ANALYST. 179 MAGNESIA OR PHOSPHORIC Acm-The triple phosphate obtained is treated in similar manner. A pure white pyro-phosphate is obtained instead of the blackish-looking mass usually got. ZINC AND CADMIonf.-when the filters containing their carbonates are burnt, an appreciable loss is sustained, particularly in the case of cadmium. The best way is to remove bulk of the precipitate, and to dissolve out remainder of zinc or cadmium with dilute nitric acid, which solution is then evaporated to dryness in a weighed dish.The chief precipitate is now added, and the whole ignited and weighed. Note by abstractor.-!l!he idea of dissolving a precipitate of the filter by means of nitric acid has already been applied in the case of zinc by Dr. S. Bein. See ANALYST, ON THE EMPLOYMENT OF DIAZO COMPOUNDS FOR THE DETECTION OF ORGANIC IM- PURITY IN WATER.-In a recent number of the Berichte der Deutschen, Chemischen GeseZZschaft (xxi., No. 9), Hr. Griess advocates the use of paradiazo-benzol-sulphuric acid for the detection of organic impurity in water. It has been known for some time that an alkaline solution of the diazo-compound gave a yellow or orange colour with human urine ; further research now shows that by this colour reaction, 1 part of human urine in 5,000 of water, and 1 part of horse urine in 50,000 parts of water can be accurately and certainly detected and estimated.100 C.C. water mixed with & C.C. human urine gave, with a few drops of the diazo solution, a colour about equal to that produced by +,,, mgr. NH, in '100 C.C. water with Nezsler's reagent. The diazo solution is made by dissolving 1 part of para-diazo-benzol-sulphuric acid in 100 parts of water, and adding NaOH solution until slightly alkaline. This solution must be used while quite fresh, as it turns yellow on keeping. The method of applying the test is very simple: to 100 C.C. water a few drops of the diazo solution are added, well mixed, and the colour produced observed. If after standing five minutes no colour forms, the water can be considered pure. It may be remarked that the colour produced by grape sugar in solution is very faint, and that diabetical urine containing 6 per cent. grape sugar gives much less colouration than normal urine. vol. xi., p. 135. L. DE K. J. B. T.
ISSN:0003-2654
DOI:10.1039/AN8881300178
出版商:RSC
年代:1888
数据来源: RSC
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9. |
Law notes. To our readers |
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Analyst,
Volume 13,
Issue 9,
1888,
Page 179-180
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摘要:
THE ANALYST. 179 ZA W NOTh’S. TO OUR READERS. Some years ago it was decided to discontinue t7~e reportiqig of ordinary police-cmrt proceedings, and onZy t o give such cases as awthoritatively established some point in connection with the working of the Acts in wvhich public analysts are interested. After a fair trial of this system, a majority of the membevs of mr Society have expressed a wish that our old practice should be, t o some extent, returned to, and, in d@erence t o such request, we have decided to resume the reporting of pvlice proceedings. The line will be dralun at accounts of ordinary cases, and reiiorts will only be inserted when any novel, legal, o(p chemical point arises, or where the certi$cate if the analyst is i 1 ~ any way attacked. A n y member or subscriber coqcnected wit7~ szccJ~ a case is, therefore, invited t o furnish us with a report of t7~e proceedings, signedwith his name, mt for publication, but as a gzcarantee of exactitude.THE ADULTERATION OF AMERICAN LABD.-Before the Potteries Stipendiary (Mr. H. C. Green- wood), at Longton, July 4th, there was an investigation of several cases involving the alleged adul- teration of lard imported from America. The cases were brought before the Court by Mr. E. W. H. Knight, inspector under the Adulteration of Food and Drugs Act ; and Mr. B’. Smith, of Liverpool, appeared for the defendants, and likewise watched the proceedings on behalf of the wholesale dealers.-In the first case, John Siddall, grocer and provision dealer, Dresden, was charged with having sold lard that was certified by the County Analyst to be adulterated to the extent of 15 per cent.with cotton-seed oil. The case was before the Court, May 30th, when it was stated that it wa8 one of the first of the kind in the country, cotton-seed oil never having been alleged as an adulteration before. At the request of Mr. Smith, a sample of the lard was ordered t o be sent to the Governmen(180 THE ANALYST. ~ ~~ laboratory at Somerset House, and the case was adjourned to await the result. It was now stated that the Government Analyst certified that the lard contained 20 per cent. of cotton-seed oi1.-Mr. Knight asked that an exemplary penalty might be imposed, as, he said, it was very evident that it was not the retailers, but the wholesale dealers who were the offenders, and were defending the matter.In support of this statement, he pointed out that the wholesale dealers had issued a circular to the retailers stating that if anything was wrong with the lard they would make it all right. This, he contended, was practically saying that they would pay any fine that might be inflicted.-Mr. Smith said that no one was more surprised than the wholesale dealers when this American lard was found to be adulterated, for until Mr. Jones (the county analyst) detected that it contained cotton-seed oil there was not an analyst in the country who could say that it was not pure. As a matter of fact some analysts had certified that it was pure. The wholesale dealers were innocent of the adultera- tion, and they therefore stood at the back, in a reasonable and proper way, of those persons whom they had innocently misled.-The Stipendiary said that he had no doubt that the adulteration was done in America, and that the defendant knew nothing about anything having been added to the lard, but, unfortunately for him, the law held him responsible.As this was one of thelfirst cases of the kind, he should treat it as a first case, but now that it was becoming known that the lard was adul- terated he should severely punish any future offenders. The defendant was fined 40s. and 19s. costs, -The following tradesmen were also charged with having sold lard adulterated with cotton-seed oil : Samuel Jenkinson, grocer, High-street, Longton, 20 per cent. ; Henry Dayson, grocer, Market-street, 17 per cent.; and Thomas Pickering, grocer, High-street, 19 per cent. The certificates of the analyst were not disputed, and the magistrate imposed a fine of 40s. and 19s. costs in each case. “ PURE AND REFINED LAED ” FROM AMERICA.-~MPORTANT PROSECUTIONS.-At the Wednes- bury Police Court, July 3rd, before the Stipendiary (Mr. Neville), George Blackham,twholesale grocer, Darlaston, was charged with selling lard not of the nature and quality demanded.-Mr. R. A. Willcock (Wolverhampton) appeared to prosecute on behalf of Mr. J. E. Morris, the Inspector under the Food and Drugs Act ; and Mr. James Slater defended.-In opening the case, Mr. Willcock stated that on June 1st Mr. Morris visited a shop at Darlaston occupied by the defendant, and there saw exposed for sale two piles of lard marked respectively 5d.and 6d. per lb. Mr. Morris asked for a pound of lard at 5d., with which Mr, Blackham supplied him, and for which Mr. Morris paid. A conversation ensued, in the course of which Mr. Blackham said he believed it was pure lard, and if it were not it was very hard that the retailer should be prosecuted.-Mr. Morris said he quite agreed with him, and a bucket was then produced, on the lid of which was printed “ Armour and Go., pure and refined lard, Chicago, U.S.”-The lard was subsequently anelysed, and was found to contain 17 per cent. of cotton- seed oil. This was first discovered by Mr. E. W. T. Jones, and the wholesale house had now recog- nised their liability, and had sent out a circular to their customers in these terms :--“Armour’s Refined Lard.-It has been decided that Armour’s refined lard, as hitherto imported from Chicago, cannot be sold as pure lard, but as mixed.We shall be happy to make any reasonable allowance that you may think needful to repay you for any temporary trouble or inconvenience you may experience in selling the mixed as distinct from the pure lard, or take back any unsold portion at your option later on should you find any trouble, which we hardly anticipate, as Messrs. Armour’s refined lard is of unimpeachable quality for domestic purposes-(laughter)-and contains the most thoroughly health- giving properties, and is extensively used by the general public all the world over.-Pelling, Stanley, and Company, Liverpool, June 20, 1888.” Together with this was a copy of label which should be supplied to every purchaser. It was “ Armour’s refined lard.This product is mixed.”-Mr. Morris having given evidence in proof of this statement, Mr. Slater for the defence said defendant purchased the lard in question as pure and refined, from Messrs. Carter and Wooding, of Liverpool, who received it from Pelling, Stanley, and Go., the agents for Messrs. Armour. To show what the profit was like, he might mention that defendant paid 42s., including carriage, for a hundredweight of lard, which was equal to 44d. per pound. He sold it at 5d. per pound, and thus only realised a profit of td. per pound,-The Stipendiary said he did not understand the prosecution to suggest that the Elnglish retail dealers got large profits. It was the Americans who were said to be doing that.-Mr.Slater then went on to contend that Mr. Blackham received a written guarantee within the meaning of the Act that the lard was pure. This, he submitted, was established by the fact that the lard- bucket lids had printed on them “Armour and Co., pure and refined lard, Chicago.”-Mr. Slater argued this point at length, but the Stipendiary said he decided that that was not a written warranty sufficient under the 25th section of the Act. So far as defendant was concerned he no doubt bought the lard as pure, and had not made much profit out of it. The profit was unfortunately got across the water.-Defendant would be fined $5 and costs, for a penalty of that kind seemed to be the only way to stop the traffic. He had not the slightest doubt defendant would be able to recover the fine, Wm. Wilkes, grocer, Darlaston, was charged with a similar offence, the lard in this case being adulterated with 19 per cent. of cotton-seed oi1.-Mr. Frederick Smith, of Liverpool, solicitor to Messrs. Pelling and Stanley, appeared for the defence, and urged that a nominal penalty would meet the case.-His Worship imposed 8 fine of 2 5 and costs, remarking that Mr. Jones had acted the Part of a public benefactor by discovering that adulteration. A good deal of profit must have been made samewhere.-Mr. Smith : It is in America.-Walter Raybold, Dudley Port, grocer, charged with a similar offence, was fined 2 6 and costs.-In the first case Mr. Slater gave notice of appeal, and the StipenEary expressed his willingness to grant him a case.-The amount of fine and costs in ea& of the cases was $6 16s. Od.
ISSN:0003-2654
DOI:10.1039/AN8881300179
出版商:RSC
年代:1888
数据来源: RSC
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