丙酮EP8.0.doc

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1、EP 8.0 各论：丙酮 01/2008:0872 (中英文）EP 7.001/2008:0872ACETONE丙酮C3H6O67-64-1 Mr 58.08【定义】Propanone丙酮。【CHARACTERS性状】Appearance: volatile, clear, colourless liquid外观：挥发性、澄清，无色液体。Solubility: miscible with water and with ethanol (96% per cent).溶解性：与水和乙醇（96%）互溶。The vapor is flammable.蒸气易燃。【IDENTIFICATION鉴别】A.

2、Relative density (see Tests)A：比重（见检查项）。B.To 1mL, add 3mL of dilute sodium hydroxide solution R and 0.3mL of a 25g/L solution of sodium nitroprusside R. An intense red colur is produced which becomes violet with the addition of 3.5mL of acetic acid R.B：于1ml样品中，加3ml稀氢氧化钠溶液（R），0.3ml的25g/L硝普钠（亚硝酰铁氰化钠）（R

3、）溶液。应呈深红色，加3.5ml醋酸（R）后变为紫色。稀氢氧化钠溶液配制方法：Sodium Hydroxide Solution, Dilute An 8.5% w/v solution of sodium hydroxide (about 2M ).硝普钠：Sodium Nitroprusside Sodium pentacyanonitrosylferrate(III) dihydrate; Na2Fe(CN)5(NO),2H2O = 298.0 (13755-38-9) Analytical reagent grade of commerce. Reddish brown powder

4、or crystals）C. To 10mL of a 0.1 per cent V/V solution of the substance to be examined in ethanol (50 per cent V/V) R, add 1mL of a 10g/L solution of nitrobenzaldehyde R in ethanol (50 per cent V/V) R and 0.5mL of strong sodium hydroxide solution R. Allow to stand for about 2 min and acidify with ace

5、tic acid R. Agreenish-blue colour is produced.C：取10ml的0.1%（V/V）样品在乙醇中（50%V/V）（R）稀释液，加1ml的10mg/L对硝基苯甲醛（R）乙醇（50%V/V）溶液，加0.5ml浓氢氧化钠溶液（R）。放置约2分钟，用醋酸（R）酸化，应显蓝绿色。浓氢氧化钠溶液（R）：Sodium Hydroxide Solution, Strong A 42% w/v solution of sodium hydroxide (about 10M ).【TESTS检查】Appearance of solution. To 10mL add 10

6、mL of water R. The solution is clear (2.2.1) and colourless (2.2.2, Method II).溶液外观：取10ml样品，加10ml水，溶液应澄清（附录2.2.1）无色（附录2.2.2，方法）。Acidity or alkalinity. To 5mL add 5mL of carbon dioxide-free water R, 0.15mL of phenolphthalein solution R and 0.5mL of 0.01M sodium hydroxide. The solution is pink. Add 0.

7、7mL of 0.01M hydrochloric acid and 0.05mL of methyl red solution R. The solution is red or orange.酸碱度：取样品5ml，加5ml无二氧化碳的水（R），0.15mL酚酞试液（R）与0.5ml的0.01M氢氧化钠，溶液显粉色。加0.7ml的0.01M盐酸，0.05ml甲基红指示液（R），溶液显红色或橙色。酚酞试液：Phenolphthalein Solution Dissolve 0.1 g of phenolphthalein R in 80 ml of alcohol R and dilute t

8、o 100 ml with water R. Complies with the following test. Test for sensitivity To 0.1 ml of the phenolphthalein solution add 100 ml of carbon dioxide-free water R. The solution is colourless. Not more than 0.2 ml of 0.02 M sodium hydroxide is required to change the colour to pink. Colour changepH 8.2

9、 (colourless) to pH 10.0 (red) 甲基红试液：Methyl Red Solution Dissolve 50 mg of methyl red in a mixture of 1.86 ml of 0.1M sodium hydroxide and 50 ml of ethanol (96%) and add sufficient water to produce 100 ml. Complies with the following test. Sensitivity A mixture of 0.1 ml of the solution, 100 ml of c

10、arbon dioxide-free water and 0.05 ml of 0.02M hydrochloric acid VS is red. Not more than 0.1 ml of 0.02M sodium hydroxide VS is required to change the colour of the solution to yellow. Colour changepH 4.4 (red) to pH 6.0 (yellow). Relative density (2.2.5): 0.790 to 0.793.比重（附录2.2.25）：0.7900.793Reduc

11、ing substances. To 30mL add 0.1mL of 0.02M potassium permanganate and allow to stand in the dark for 2h. The mixture is not completely decolorized.还原性物质：取样品30ml，加0.1ml的0.02m高锰酸钾，在黑暗中放置2小时，混合物不得全褪色。Related substances. Gas chromatography (2.2.28).有关物质：气相（附录2.2.28）Test solution. The substance to be exa

12、mined.供试液：待检样品Reference solution (a). To 0.5mL of methanol R add 0.5mL of 2-propanol R and dilute to 100.0mLwith the test solution. Dilute 1.0mL of this solution to 10.0mL with the test solution.对照液（a）：取0.5ml异丙醇（R）加于0.5ml甲醇（R）中，用供试液稀释至100.0ml。移取1.0ml用供试液稀释至10.0ml。Reference solution (b). Dilute 100uL

13、 of benzene R to 100.0mL with the test solution. Dilute 0.20mL of this solution to 100.0mL with the test solution.对照液（b）：取100L苯（R）于100.0mL容量瓶，用供试液稀释至刻度。移取0.20ml该溶液用供试液稀释至100.0ml。Column: 色谱柱：-material: fused silica,色谱柱材料：熔融石英-size: l=50m, D=0.3mm尺寸：l=50m，D=0.3mm-stationary phase: macrogol 20,000R (fi

14、lm thickness 1um).固定相：聚乙二醇20000R（膜厚 1m）Carrier gas: helium for chromatography R.载气：高纯氦气（Helium He = 4.003 (7440-59-7) Laboratory cylinder grade of commerce containing not less than 99.995% v/v of He）. Linear velocity: 21cm/s.线速度：21cm/sSplit ration:1:50分流比：1：50Temperature 升温程序Time 时间（min 分钟）Temperatu

15、re 温度（）Column 柱温0-114510011-20100Injection port进样口150Detector 检测器250Detection: flame ionization.检测器：FID Injection: 1uL.进样量：1LRetention time: impurity C = about 7.5min保留时间：杂质C（苯）=约7.5分钟System suitability: 系统适用性：-resolution: minimum 5.0 between the peak due to impurity A (2nd peak) and the peak due to

16、 impurity B (3rd peak) in the chromatogram obtained with reference solution (a).分离度：对照液（a）中杂质A（第2个峰）与杂质B（第3个峰）分离度不小于5.0-signal-to-noise ration: minimum 5 for the peak due to impurity C in the chromatogram obtained with reference solution (b).信噪比：对照液（b）色谱图中杂质C（苯）的信噪比不小于5。Limits: 限度-impurities A, B: f

17、or each impurity, not more than the difference between the areas of the corresponding peaks in the chromatogram obtained with reference solution (a) and the areas of the corresponding peaks in the chromatogram obtained with the test solution (0.05 per cent V/V).杂质A，B：各杂质峰面积不大于对照液（a）色谱图中相应峰面积与供试液色谱图中

18、对应峰面积差值（0.05%V/V）-impurity C: not more than the difference between the area of the peak due to impurity C in the chromatogram obtained with reference solution (b) and the area of the corresponding peak in the chromatogram obtained with the test solution (2ppm V/V).杂质C（苯）：杂质C面积不大于对照液（b）色谱图中杂质C峰面积与供试液

19、色谱图中杂质C面积差值（2ppmV/V）-any other impurity: for each impurity, not more than the difference between the area of the peak due to impurity A in the chromatogram obtained with reference solution (a) and the area of the corresponding peak in the chromatogram obtained with the test solution (0.05 per cent V

20、/V).-其它单一杂质：各杂质面积不大于对照液（a）色谱图中杂质A峰面积与供试液色谱图中相应峰面积之差值（0.05%V/V）Matter insoluble in water Dilute 1.0mL to 20mL with water R. The solution is clear (2.2.1)水不溶物取1.0ml样品，用水稀释至20ml，溶液应澄清（附录2.2.1）。Residue on evaporation: maximum 50ppm.蒸发残渣：不得过50ppmEvaporate 20.0g to dryness on a water-bath and dry at 100-1

21、05. The residue weighs a maximum of 1mg.取样品20.0g，水浴加热至干，100-105干燥，残渣不超过1mg。Water (2.5.12): maximum 3g/L. determined on 10.0mL. Use 20mL of anhydrous pyridine R as solvent.水分（附录2.5.12）：不得过3g/L取样品10.0ml，用20ml无水吡啶（R）为溶剂，滴定。【STORAGE贮存】Protected from light.避光保存。【IMPURITIES杂质】A CH3-OH: methanol. 杂质A：甲醇B. CH3-CHOH-CH3: propan-2-ol (isopropanol) 杂质B：异丙醇C: C6H6: Benzene. 杂质C：苯译者注：文中的“（R）”表示EP 规定的试剂级别