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CRS | Dichlorophenolindophenol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)】 |
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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.