SACCHARINE PRODUCTS. 69 



(d) ALKALINITY OF SOLUBLE ASH. PROVISIONAL. 



Allow the filtrate from the above determination to cool, then titrate with tenth- 

 normal hydrochloric acid, using methyl orange as an indicator. 



(e) ALKALINITY OF INSOLUBLE ASH. PROVISIONAL. 



Add excess of tenth-normal hydrochloric acid (usually 10 to 15 cc) to the 

 ignited insoluble ash in the platinum dish, heat to the point of boiling over an 

 asbestos plate, allow to cool, and titrate excess of hydrochloric acid with tenth- 

 normal sodium hydroxid, using methyl orange as an indicator. 



Express the alkalinity in each case as the number of cubic centimeters of 

 tenth-normal acid used on the ash of 1 gram of sample. 



(f) MINERAL ADULTERANTS IN ASH. 



(1) REDUCTION TO ASH. PROVISIONAL. 



Comparatively large quantities of saccharine products may be readily and 

 quickly reduced to an ash for mineral examination without the troublesome 

 frothing that ordinarily ensues in igniting at once with a free flame by proceed- 

 ing as follows : 



Mix 100 grams of molasses, sirup, or honey, or of the confectionery solution 

 (b) under " 1. Preparation of Sample," p. 64, evaporated to a sirupy consist- 

 ency, with about 35 grams of concentrated sulphuric acid in a large porcelain 

 evaporating dish. Then pass an electric current through it while stirring by 

 placing one platinum electrode in the bottom of the dish near one side and at- 

 taching the other to the lower end of the glass rod with which the contents are 

 stirred. Begin with a current of about 1 ampere and gradually increase to 

 4.& In from ten to fifteen minutes the mass is reduced to a fine dry char, which 

 may then be readily burnt to a white ash in the original dish over a free flame 

 or in a muffle. 



If an electric current is unavailable, treat in a large porcelain dish 100 grams 

 of the saccharine solution to be ashed, which should be evaporated to a sirupy 

 consistency if not already in such condition, with sufficient concentrated sul- 

 phuric acid to throughly carbonize the mass, after which ignite in the usual 

 manner. 



Among the suspected adulterants to be looked for in the ash are salts of 

 tin, used in molasses to bleach or lighten the color; mineral pigments, such as 

 chroinate of lead in yellow confectionery and oxid of iron, the latter being 

 sometimes used as an intensifier of or substitute for the natural color of 

 chocolate. 



(2) TIN IN MOLASSES <? AND OTHER SACCHARINE PRODUCTS.* PROVISIONAL. 



Fuse the ash from a weighed portion of the sample with sodium hydroxid in 

 a silver crucible, dissolve in water, and acidulate with hydrochloric acid ; 



Leach, Thirty-second Ann. Rept. Mass. State Board of Health, 1900, p. 653 ; reprint, 

 p. '!". This method is preferred to the ordinary method of heating with sulphuric acid, 

 especially in the case of molasses, because, if properly manipulated, it comes quietly into 

 the form of a very finely divided char or powder, especially adapted for subsequent quick 

 ignition. 



6 Modified from method of Budde and Schou for determining nitrogen electrolytically. 

 Zts. anal. Chem., 1899, 38: 345. 



c Leach, Thirty -second Ann. Rept. Mass. State Board of Health, 1899, p. 625; Hilger 

 and Laband, Zts. Nahr. Genussm., 1899, 2: 795. 



* This method is applicable also to condensed milk, canned goods, etc. 



e See page 61, under " IX. Canned Vegetables," section 7. 



