USP附录般鉴别试验.docx

1、USP 附录般鉴别试验附录般鉴别试验 USP38 附录一般鉴别试验 作者：日期：USP32 附录 191一般鉴别试验：主要的问题是里面的一些英文 and是翻译成“和”还是“或”Under this heading are placed tests that are frequently referred to in the Pharmacopeia for the identification of official articles.Before using any acid or base to modify the PH of the sample solution,make sure

2、that the added substance will not interfere with the results of the test.NOTEThe tests are not intended to be applicable to mixtures of substances unless so specified.此处列举的检查项目都是频繁应用于药典鉴别项下的内容.在用任何酸或基础物质调整样品溶液的 PH前,要保证所加的物质不会影响到检测结果：（注:除另有规定外，不适用于混合物)Acetate-Dissolve about 30mg of the substance to b

3、e examined in 3ml of the prescribed solution.Adjust the PH of the solution with sodium hydroxide to slightly alkaline。Add 0.25ml of lanthanum nitrate TS.If a white precipitate is formed,filter the solution.Add successively 0.1ml of iodine and potassium iodide TS 3 and 0.1ml of ammonia TS 2 to the so

4、lution.I f no blue color is observed，heat carefully to boiling.In the presence of acetates，a dark color develops or a blue precipitate is fprmed。With neureal solutions of acetates,ferric chloride TS produces a red color tha is destroyed by the addition of mineral acids.个人收集整理，勿做商业用途 醋酸盐：硝酸镧试液。如出现白色沉

5、淀，过滤溶液。先后加入 0。1ml 的碘和碘化钾试液 3和 0。1ml 的氨试液至溶液中。如没得到蓝色，小心加热至沸腾。如硝酸盐出现深色或蓝色沉淀物.取醋酸的中性溶液，加三氯化铁试液出现红色,加无机酸，红色破坏.Aluminum With 6 N ammonium hydroxide,solutions of aluminum salts yield a gelatinous,white precipitate that is insoluble in an excess of 6 N ammonium hydroxide。1 N sodium hydroxide or sodium sulf

6、ide TS produces the same precipitate,which dissolves in an excess of either of these reagents。铝:1、加入 6N的氨水,应产生白色胶状沉淀，沉淀物在过量的 6N的氨水中不溶。2、加入 1N的氢氧化钠或硫化钠试液，应产生白色胶状沉淀，当上述试液过量时，沉淀应溶解。Ammonium Add 0.2g of magnesium oxide to the solution under test.Pass a current of air through the mixture，and direct the g

7、as that escapes to just beneath the surface of an indicator solution,prepared by mixing 1ml of 0.1M hydrochloric acid and 0.05ml of methyl red TS2。In the presence of ammonium，the color of the indicator solution is changed to yellow.After directing the gas into the indicator solution for a sufficient

8、 period of time，add 1ml of freshly prepared sodium cobaltinitrite TS to the indicator solution。Upon the addition of the sodium cobaltinitrite TS，a yellow precipitate is formed when ammonium is present。个人收集整理，勿做商业用途 铵：溶液中加入 0。2g氧化镁。混合物产生气体，把产生的气体通入指示剂的液面下，（指示剂配制：1ml0。1M 盐酸和 0。05ml 的甲基红试液 2。）指示液变黄色。气体

9、通入指示液充分后，加入 1ml 新配的亚硝酸钴钠试液。由于亚硝酸钴钠试液的加入,铵会出现黄色沉淀物。Antimony With hydrogen sulfide，solutions of antimony（III)compounds，strongly acidified with hydrochloric acid，yield an orange precipitate of antimony sulfide that is insoluble in 6 N ammonium hydroxide，but is soluble in ammonium sulfide TS.锑:三价锑溶液加盐酸酸

10、化后，通硫化氢，应产生橘红色硫化锑沉淀,沉淀不溶于6N的氨水,可溶于硫化铵试液。Barium Solutions of barium salts yield a white precipitate with 2N sulfuric acid.This precipitate is insoluble in hydrochloric acid and in nitric acid.Barium salts impart a yellowish-green color to a nonluminous flame that appears blue when viewed through gree

11、n glass.钡:1、加 2N硫酸,钡盐溶液产生白色沉淀。沉淀在盐酸和硝酸中不溶。2、钡盐于无色光焰中发出淡黄绿光,透过绿色玻璃观察应为蓝色。Benzoate In neutral solutions,benzoates yield a salmon-colored precipitate with ferric chloride TS.In moderately concentrated solutions,benzoates yield a precipitate of benzoic acid upon acidification with 2N sulfuric acid.This

12、precipitate is readily soluble in ethyl ether.苯甲酸盐:1、苯甲酸盐的中性溶液与三氯化铁试液反应产生赭色沉淀。2、苯甲酸盐的浓溶液被 2N的硫酸酸化后应产生苯甲酸沉淀，沉淀在乙醚中易溶.Bicarbonate-See Carbonate.碳酸氢盐：参照碳酸盐 Bismuth When dissolved in a slight excess of nitric acid or hydrochloric acid，bismuth salts yield a white precipitate upon dilution with water.This

13、 precipitate is colored brown by hydrogen sulfide，and the resulting compound dissolves in a warm mixture of equal parts of nitric acid and water.铋:铋盐的水稀释液加入稍过量的硝酸或者盐酸，应产生白色沉淀.沉淀加入硫化氢后变为棕色，产物溶于温热的硝酸溶液（硝酸：水=1:1）。Bisulfite See Sulfite.亚硫酸氢盐：参照硫酸盐。Borate To 1 mL of a borate solution,acidified with hydro

14、chloric acid to litmus,add 3 or 4 drops of iodine TS and 3 or 4 drops of polyvinyl alcohol solution(1 in 50)：an intense blue color is produced.When a borate is treated with sulfuric acid,methanol is added，and the mixture is ignited,it burns with a greenbordered flame。硼酸盐:1、1ml 硼酸盐溶液用盐酸酸化至对石蕊试纸显酸性,加入

15、 34滴碘试液和3-4 滴聚乙烯醇溶液(1：50)，溶液应显深蓝色。2、硼酸盐溶于硫酸，加入甲醇后点燃,火焰边缘应为绿色。Bromide Solutions of bromides,upon the addition of chlorine TS，dropwise,liberate bromine,which is dissolved by shaking with chloroform,coloring the chloroform red to reddish brown.Silver nitrate TS produces in solutions of bromides a yello

16、wishwhite precipitate that is insoluble in nitric acid and is slightly soluble in 6N ammonium hydroxide。溴化物：1、溴化物溶液逐滴加入氯试液，游离出溴，用氯仿萃取，氯仿层应为红棕色.2、溴化物溶液中加入硝酸银试液，应产生浅黄色絮乳状沉淀，沉淀不溶于硝酸，微溶于 6N的氨水.Calcium Solutions of calcium salts form insoluble oxalates when treated as follows。To a solution of the calcium

17、 salt(1 in 20）add 2 drops of methyl red TS,and neutralize with 6N ammonium hydroxide.Add 3N hydrochloric acid，dropwise,until the solution is acid to the indicator.Upon the addition of ammonium oxalate TS,a white precipitate is formed。This precipitate is insoluble in 6N acetic acid but dissolves in h

18、ydrochloric acid。Calcium salts moistened with hydrochloric acid impart a transient yellowishred color to a nonluminous flame.文档为个人收集整理，来源于网络 钙：按以下方式钙盐溶液形成不溶的草酸盐。钙盐溶液（120）中加入 2 滴甲基红试液，用 6N的氨水中和，缓缓滴加 3N的盐酸使其恰成酸性。加入草酸铵试液,应生成白色沉淀。沉淀不溶于 6N乙酸，溶于盐酸。用盐酸润湿的钙盐在无色光焰中应呈砖红色。Carbonate-Carbonates and bicarbonates

19、effervesce with acids，evolving a colorless gas that,when passed into calcium hydroxide TS,produces a white precipitate immediately。A cold solution(1 in 20)of a soluble carbonate is colored red by phenolphthalein TS，while a similar solution of a bicarbonate remains unchanged or is only slightly color

20、ed.碳酸盐：1、碳酸盐与碳酸氢盐遇酸，剧烈反应，产生无色气体，通入氢氧化钙溶液中，立即产生白色沉淀.2、可溶性冷的碳酸盐溶液（120)加入酚酞试液显红色，同浓度的碳酸氢盐也呈现红色或略浅的红色。Chlorate Solutions of chlorates yield no precipitate with silver nitrate TS。The addition of sulfurous acid to this mixture produces a white precipitate that is insoluble in nitric acid,but is soluble in

21、 6N ammonium hydroxide.Upon ignition，chlorates yield chlorides，recognizable by appropriate tests.When sulfuric acid is added to a dry chlorate,decrepitation occurs，and a greenish yellowgas is evolved。CautionUse only a small amount of chlorate for this test，and exercise extreme caution in performing

22、it.文档为个人收集整理，来源于网络 氯酸盐：1、氯酸盐溶液加入硝酸银试液不会出现沉淀，当加入亚硫酸后,混合物产生白色沉淀，沉淀不溶于硝酸,可溶于 6N的氨水。2、用适当的方法表明氯酸盐经点燃应产生氯化物.3、在干燥的氯酸盐上滴加硫酸，剧烈反应，并产生黄绿色气体。(警告：进行此试验应使用极小量氯酸盐，且操作时要谨慎小心。）Chloride With silver nitrate TS,solutions of chlorides yield a white,curdy precipitate that is insoluble in nitric acid but is soluble in

23、a slight excess of 6N ammonium hydroxide.When testing amine(including alkaloidal）hydrochlorides that do not respond to the above test,add one drop of diluted nitric acid and 0。5 mL of silver nitrate TS to a solution of the substance being examined containing,unless otherwise directed in the monograp

24、h，about 2mg of chloride ion in 2mL:a white,curdy precipitate is formed。Centrifuge the mixture without delay,and decant the supernatant layer.Wash the precipitate with three 1mL portions of nitric acid solution（1 in 100），and discard the washings。Add ammonia TS dropwise to this precipitate.It dissolve

25、s readily。When a monograph specifies that an article responds to the test for dry chlorides，mix the solid to be tested with an equal weight of manganese dioxide,moisten with sulfuric acid，and gently heat the mixture:chlorine，which is recognizable by the production of a blue color with moistened star

26、ch iodide paper,is evolved.文档为个人收集整理，来源于网络 氯化物:1、加入硝酸银试液，可产生白色凝乳状沉淀,沉淀不溶于硝酸，但可溶于稍过量的 6N氨水.2、如果测试胺类盐酸盐（包括生物碱类）不能如上述反应，除另有规定外，准备供试品溶液 2ml（约含 2mg氯离子），加入 1滴稀硝酸和 0。5ml 硝酸银试液,应出现白色凝乳状沉淀，立即离心,弃去上清液，沉淀分 3 次用 1ml 硝酸溶液(1100）洗涤，弃去洗涤液。逐滴滴加氨试液，沉淀即溶解。3、将供试品与二氧化锰等量混合，用硫酸润湿，缓缓加热，应产生氯气，使湿润的淀粉碘化钾试纸变蓝,该方法只能用于专论中干燥的固体氯

27、化物实验。Citrate-To 15mL of pyridine add a few mg of a citrate salt,dissolved or suspended in 1 mL of water，and shake.To this mixture add 5 mL of acetic anhydride,and shake：a light red color is produced.柠檬酸盐：取数毫克柠檬酸盐溶解或悬浮在 1ml 水中，加入 15ml 吡啶，振摇,再加入 5ml 醋酐,振摇，溶液应显淡红色.Cobalt Solutions of cobalt salts（1 in

28、20)in 3 N hydrochloric acid yield a red precipitate when heated on a steam bath with an equal volume of a hot，freshly prepared solution of 1nitroso2-naphthol（1 in 10)in 9 N acetic acid.Solutions of cobalt salts，when saturated with potassium chloride and treated with potassium nitrite and acetic acid

29、，yield a yellow precipitate.钴：1、钴盐的 3N 盐酸溶液（120）与等体积新配的热 1-硝基 2萘酚的 9N的醋酸溶液（110）混合，在蒸气浴中，应产生红色沉淀.2、钴盐溶液用氯化钾饱和，经亚硝酸钾和醋酸处理,应产生黄色沉淀。Copper Solutions of cupric compounds,acidified with hydrochloric acid,deposit a red film of metallic copper upon a bright，untarnished surface of metallic iron。An excess of

30、6N ammonium hydroxide,added to a solution of a cupric salt,produces first a bluish precipitate and then a deep bluecolored solution。With potassium ferrocyanide TS,solutions of cupric salts yield a reddish-brown precipitate，insoluble in diluted acids。个人收集整理，勿做商业用途 铜：1、供试品溶液经盐酸酸化后，放入表面光滑明亮的金属铁，在铁表层应形成

31、一层红色的金属铜膜。2、铜盐溶液中加入过量的 6N的氨水，先产生淡蓝色(青白色）沉淀,沉淀逐渐变为深蓝色。3、供试品与亚铁氰化钾试液反应生成红褐色沉淀，沉淀不溶于稀酸.Hypophosphite When strongly heated，hypophosphites evolve spontaneously flammable phosphine。Hypophosphites in solution yield a white precipitate with mercuric chloride TS.This precipitate becomes gray when an excess o

32、f hypophosphite is present.Solutions of hypophosphites，acidified with sulfuric acid，and warmed with cupric sulfate TS yield a red precipitate。文档为个人收集整理，来源于网络 次磷酸盐:1、次磷酸盐加强热，产生磷化氢，并能自燃。2、供试品溶液中加入氯化汞试液，产生白色沉淀,当供试品过量时,沉淀颜色变为灰色。3、供试品溶液用硫酸酸化后,加入硫酸铜试液,温热,产生红色沉淀。Iodide Solutions of iodides，upon the additio

33、n of chlorine TS，dropwise，liberate iodine,which colors the solution yellow to red.When the solution is shaken with chloroform,the latter is colored violet。The iodine thus liberated gives a blue color with starch TS.Silver nitrate TS produces,in solutions of iodides，a yellow,curdy precipitate that is insoluble in nitric acid and in 6N ammonium hydroxide.本文为互联网收集，请勿用作商业用途 碘化物：1、碘化物溶液中逐滴滴加氯试液，碘析出，溶液颜