XXIV. SPICES AND OTHER CONDIMENTS. 



SPICES. 



1 PREPARATION OF SAMPLE.— TENTATIVE. 



Grind the sample so as to pass through a sieve having circular openings 1 mm. in 

 diameter and mix thoroughly. Owing to the lack of uniformity of most spices 

 and the peculiar tendency to stratify, extreme care is necessary in weighing out a 

 portion for analysis. Stir the material with a spoon, having a capacity of approxi- 

 mately 2 grams, and dip a spoonful from the interior in order that only a very small 

 amount needs to be added to or taken from the portion on the scale pan. In the 

 determination of starch in spices by the diastase method, reduce a portion of the 

 sample to an impalpable powder by grinding in a mortar. 



2 MOISTURE.— TENTATIVE. 



Dry 2 grams to constant weight at 110°C. From the resulting loss in weight 

 subtract the amount of volatile ether extract as determined in 9. 



3 ASH.— OFFICIAL. 

 Determine as directed under VIII, 4. 



4 SOLUBLE AND INSOLUBLE ASH.— TENTATIVE. 

 Proceed as directed under IX, 17, employing the ash obtained in 3. 



5 ASH INSOLUBLE IN ACID.— TENTATIVE. 



Boil the water-insoluble residue, obtained in 4, or the total ash obtained in 3, 

 with 25 cc. of 10% hydrochloric acid (sp. gr. 1.050) for 5 minutes, collect the insol- 

 uble matter on a Gooch or an ashless filter, wash with hot water, ignite and weigh. 



6 CALCIUM OXID IN ASH.— OFFICLAL. 



Ignite 2-A grams of the sample as directed under 3, digest with hot 10% hydro- 

 chloric acid, evaporate to dryness, moisten the dry residue with dilute hydro- 

 chloric acid and again evaporate to drjmess to render the silica insoluble. Moisten 

 the residue with 5-10 cc. of hydrochloric acid, add about 50 cc. of water, allow to 

 stand on a water bath for a few minutes, filter and wash the insoluble residue with 

 hot water. Determine calcium oxid in the combined filtrate and washings as directed 

 under XXVIII, 23. 



7 NITROGEN.— OFFICIAL. 



Determine as directed under I, 18, 21 or 23, except in the case of black and 

 white peppers in which use only the Kjeldahl-Gunning-Arnold method' [I, 23], 

 employing 1 gram of the sample. 



NITROGEN IN NON-VOLATILE ETHER EXTRACT. 



8 Wititon, Ogden and Mitchell Method. — Tentative. 



(For black and white peppers.) 



Extract 10 grams of the pepper for 20 hours in a continuous extraction apparatus 

 with absolute ether, collecting the extract in a weighed 250 cc. flask. Evaporate 



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