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【分享】EP6.0 3.1.3 Polyolefines中所用到的试剂清单

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  • 有版友需要EP6.0关于3.1.3 Polyolefines中所用到的一些试剂清单,这个章节里面所涉及到的试剂很多,下面列出了一些,可能有漏掉的,欢迎大家补充。另外附加测试中还有一些塑料添加剂的化学参照物质没有列出来,附加测试可根据物料成分进行选择性地检测。



    Toluene甲苯Phosphoric acid磷酸
    Potassium hydrogen sulphate硫酸氢钾Potassium permanganate高锰酸钾
    Methylene chloride二氯甲烷Trimethylpentane三甲基戊烷
    Methanol 甲醇Hydrochloric acid盐酸
    Starch淀粉Methyl orange甲基橙
    2-Propanol异丙醇Acetonitrile乙腈
    titanium dioxide二氧化钛Sodium thiosulphate硫代硫酸钠
    Hydrogen peroxide过氧化氢Phosphomolybdic acid磷钼酸
    Sulphuric acid硫酸Hexane正已烷
    Tetrahydrofuran四氢呋喃Potassium iodide碘化钾
    Sodium hydroxide氢氧化钠Tetrabutylammonium hydroxide四丁基氢氧化铵
    Butylhydroxytoluene丁基羟基甲苯CRSDichlorophenolindophenol二氯酚靛酚
    BRP指示液(由溴麝香草酚蓝bromothymol blue、甲基红methyl red、酚酞phenolphthalein及乙醇 Ethanol配制而成)
    Tert-butylhydroperoxide叔丁基化过氧氢【1,1-Dimethylethylhydroperoxide; C4H10O2 = 90.1 (75-91-2)


    下面是部分英文原文:

    Identification

    If necessary, cut samples of the material to be examined into pieces of maximum dimension on a side of not greater than 1 cm.

    A. To 0.25 g add 10 ml of toluene R and boil under a reflux condenser for about 15 min. Place a few drops of the solution obtained on a sodium chloride slide and evaporate the solvent in an oven at 80 °C. Examine by infrared absorption spectrophotometry (2.2.24). The spectrum of the material to be examined shows maxima in particular at some of the following wave-numbers: 2920 cm-1, 2850 cm-1, 1475 cm-1, 1465 cm-1, 1380 cm-1, 1170 cm-1, 735 cm-1, 720 cm-1; the spectrum obtained is identical to the spectrum obtained with the material selected for the type sample. If the material to be examined is in the form of sheets, the identification may be determined directly on a cut piece of suitable size.

    B. It complies with the supplementary tests corresponding to the additives present.

    C. In a platinum crucible, mix about 20 mg with 1 g of potassium hydrogen sulphate R and heat until completely melted. Allow to cool and add 20 ml of dilute sulphuric acid R. Heat gently. Filter the resulting solution. To the filtrate add 1 ml of phosphoric acid R and 1 ml of strong hydrogen peroxide solution R. If the substance is opacified with titanium dioxide, an orange-yellow colour develops.

    Tests

    If necessary, cut samples of the material to be examined into pieces of maximum dimension on a side of not greater than 1 cm.

    Solution S1 Use solution S1 within 4 h of preparation. Place 25 g in a borosilicate-glass flask
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    第1楼2010/04/29

    with a ground-glass neck. Add 500 ml of water for injections R and boil under a reflux condenser for 5 h. Allow to cool and decant. Reserve a portion of the solution for the test for appearance of solution S1 and filter the rest through a sintered-glass filter (16).

    Solution S2 Place 2.0 g in a conical borosilicate-glass flask with a ground-glass neck. Add 80 ml of toluene R and boil under a reflux condenser with constant stirring for 90 min. Allow to cool to 60 °C and add with continued stirring 120 ml of methanol R. Filter the solution through a sintered-glass filter (16). Rinse the flask and the filter with 25 ml of a mixture of 40 ml of toluene R and 60 ml of methanol R, add the rinsings to the filtrate and dilute to 250 ml with the same mixture of solvents. Prepare a blank solution.

    Solution S3 Place 100 g in a conical borosilicate-glass flask with a ground-glass neck. Add 250 ml of 0.1 M hydrochloric acid and boil under a reflux condenser with constant stirring for 1 h. Allow to cool and decant the solution.

    Appearance of solution S1 Solution S1 is clear (2.2.1) and colourless (2.2.2, Method II).

    Acidity or alkalinity To 100 ml of solution S1, add 0.15 ml of BRP indicator solution R. BRP Indicator Solution Dissolve 0.1 g of bromothymol blue, 20 mg of methyl red and 0.2 g of phenolphthalein in sufficient ethanol (96%) to produce 100 ml; filter. Not more than 1.5 ml of 0.01 M sodium hydroxide is required to change the colour of the indicator to blue. To 100 ml of solution S1 add 0.2 ml of methyl orange solution R. Not more than 1 ml of 0.01 M hydrochloric acid is required to initiate the colour change of the indicator from yellow to orange.

    Absorbance (2.2.25) At wavelengths from 220 nm to 340 nm, the absorbance of solution S1 is not greater than 0.2.

    Reducing substances To 20 ml of solution S1 add 1 ml of dilute sulphuric acid R and 20 ml of 0.002 M potassium permanganate. Boil under a reflux condenser for 3 min and cool immediately. Add 1 g of potassium iodide R and titrate immediately with 0.01 M sodium thiosulphate, using 0.25 ml of starch solution R as indicator. Carry out a blank titration. The difference between the titration volumes is not more than 3.0 ml.

    Substances soluble in hexane Place 10 g in a 250 ml conical borosilicate-glass flask with a ground-glass neck. Add 100 ml of hexane R and boil under a reflux condenser for 4 h, stirring constantly. Cool in iced water and filter rapidly (the filtration time must be less than 5 min; if necessary the filtration may be accelerated by applying pressure to the solution) through a sintered-glass filter (16) maintaining the solution at about 0 °C. Evaporate 20 ml of the filtrate in a tared borosilicate-glass dish on a water-bath. Dry the residue in an oven at 100-105 °C for 1 h. The mass of the residue obtained must be within 10 per cent of that of the residue obtained with the type sample and does not exceed 5 per cent.

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    Extractable aluminium Not more than 1 ppm of extractable Al, determined by atomic emission spectrometry in an argon plasma (2.2.22, Method I).

    Test solution Use solution S3.

    Reference solutions Prepare the reference solutions using aluminium standard solution (200 ppm Al) R, diluted with 0.1 M hydrochloric acid.

    Carry out the determination using the emission of aluminium at 396.15 nm, the spectral background being taken as 396.25 nm.

    Verify the absence of aluminium in the hydrochloric acid used.

    Extractable titanium Not more than 1 ppm of extractable Ti, determined by atomic emission spectrometry in an argon plasma (2.2.22, Method I).



    Test solution Use solution S3.

    Reference solutions Prepare the reference solutions using titanium standard solution (100 ppm Ti) R, diluted with 0.1 M hydrochloric acid.

    Carry out the determination using the emission of titanium at 336.12 nm, the spectral background being taken as 336.16 nm.

    Verify the absence of titanium in the hydrochloric acid used.

    Extractable zinc Not more than 1 ppm of extractable Zn, determined by atomic absorption spectrometry (2.2.23, Method I).

    Test solution Use solution S3.

    Reference solutions Prepare the reference solutions using zinc standard solution (10 ppm Zn) R, diluted with 0.1 M hydrochloric acid.

    Measure the absorbance at 213.9 nm using a zinc hollow-cathode lamp as a source of radiation and an air-acetylene flame.

    Verify the absence of zinc in the hydrochloric acid used.

    Extractable heavy metals (2.4.8) Evaporate 50 ml of solution S3 to about 5 ml on a water-bath and dilute to 20.0 ml with water R. 12 ml of the solution complies with limit test A for heavy metals (2.5 ppm). Prepare the standard using 2.5 ml of lead standard solution (10 ppm Pb) R.

    Sulphated ash (2.4.14) Not more than 1.0 per cent, determined on 5.0 g. This limit does not apply to material that has been opacified with titanium dioxide.

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