Alcohol Specifications

Japan

Japanese Industrial Standard K 8101 - 1987

Anhydrous Ethanol

Ethanol (99.5) / Ethyl Alcohol (99.5)

C2H5OH     M.W. : 46.07

Note: This standard is an edited, abridged version of the standard. It includes extensive changes and corrections of the original, official translation, to make it more intelligible. For full details, reference should be made to the original standard, which is available from the Japanese Standards Association, Tokyo.

 

  1. Scope:

    This Japanese Industrial Standard refers to ethanol (99.5) to be used as a reagent.
  2. Physical properties:

    The sample should be a colorless, transparent and volatile liquid, soluble in water, diethyl-ether, chloroform and benzene. The boiling point is about 78°C.
  3. Identifying reactions:
    a) When 1 ml of sample is added to 1 ml of sodium hydroxide solution (30 w/v %) and 10 ml of 0.05 mol/0.1 N iodine solution, a faint yellow turbidity is generated.

    b) When 0.2 ml of ethanol sample is mixed with 5 ml of 20 % sulfuric acid  and 1 ml of 5 % w/v potassium dichromate solution and heated in water bath, a bluish green color develops.

    c) When the infrared absorption spectra are measured in accordance with J.I.S. K. 0117, the main absorptions should be in the vicinity of wavelengths 3340 cm-1, 2985 cm-1,1450 cm-1, 1380 cm-1, 1090 cm-1, 1050 cm-1 and 880 cm-1.

  4. Grades:

    The two grades of ethanol, when tested according to the methods set out in section 5.1 and 5.2, shall meet the following specifications:
    Test Premium grade Grade 1
    Miscibility in water Within the limits Within the limits
    Specific gravity (20/20°C) 0.793 max. 0.793 max.
    Water content % 0.4 (4,000 p.p.m) max. 0.4 (4,000 p.p.m) max.
    Non-volatile matter % 0.001 (10 p.p.m) max. 0.003 (30 p.p.m) max.
    Acids, as acetic acid Within the limits
    Approx. 0.002 % 
    (20 p.p.m) max.    		 Within the limits
    Approx. 0.002 % 
    (20 p.p.m) max.
    Alkalis, as ammonia Within the limits
    Approx. 0.0001 % 
    (1 p.p.m) max.    		 Within the limits
    Approx. 0.0001 %
     (1 p.p.m) max.
    Heavy metals, as Pb % 0.0001  (1 p.p.m) max. 0.0002  (2 p.p.m) max.
    Aldehydes and ketones, 
    as acetaldehyde    		 Within the limits
    Approx. 0.001 % 
    (10 p.p.m) max.    		 Within the limits
    Approx. 0.001 % 
    (10 p.p.m) max.
    Fusel oils, as pentanol 0.004 % (40 p.p.m) max. 0.004 % (40 p.p.m) max.
    Methanol 0.02 % (200 p.p.m) max. 0.02 % (200 p.p.m) max.
    Benzene and other organic 
    impurities, as benzene    		 Within the limits
    Approx. 0.005 % 
    (50 p.p.m) max.    		 Within the limits
    Approx. 0.005 % 
    (50 p.p.m) max.
    Permanganate reducing 
    substances, as oxygen equivalent    		 Within the limits
    Approx 0.0003 %
    (3 p.p.m) max.    		 Within the limits
    Approx. 0.0003 % 
    (3 p.p.m) max.
    Sulfuric acid coloring substances Within the limits Within the limits
    Ethanol content (by specific gravity) 99.5 % min. 99.5 % min.

Note: The Parts per Million (p.p.m) figures in parentheses do not appear in the original standard, but have been inserted to facilitate comparison with other standards.

  1. TEST METHODS:

    5.1. PREMIUM GRADE: Test methods for this grade are as follows:
    1. Water miscibility Mix 10 ml of the sample in 30 ml of water, and test it in accordance with method 5.2 of JIS K 8001. The mixture should be transparent after standing for one hour.
    2. Specific gravity (20/20°C) The specific gravity shall be measured in accordance with method 3.2.1 of JIS K 0061.
    3. Water Content Test 10 g of the sample in accordance with method 2.1 (4) (a) (ii) of JIS K 0068.
    4. Non-volatile matter Test 100 g of the sample in accordance with method 2.3.1 (2) of JIS K 0067. The amount of residue shall be not more than 1 mg. (The residue can be used for the test of heavy metals).
    5. Acid and alkali Test 20 ml of the sample in accordance with 5.6 (1) of JIS K 8001 using water free of carbon dioxide.
    6. Heavy metals, as Pb Add 1 ml of hydrochloric acid to the residue form test 4 (for non-volatile matter) and evaporate to dryness on a water bath, then add 1 ml of hydrochloric acid and dilute with water to 30 ml. Take 15 ml of this solution and test it in accordance with 5.24 (1) of JIS K 8001.
    7. Aldehydes and ketones Dilute 5 ml of the sample with water to 10 ml, and add 1 ml of 2,4-dinitrophenylhydrazine solution into 1 ml of this mixture. Heat it in a water bath at about 50°C for 30 min, and then after cooling it, add 5 ml of ethanolic potassium hydroxide solution. After 5 min standing, compare this color with the color obtained as follows: Take 4 ml of standard acetone solution (0.01 mg CH3COCH3/ml) and add 5 ml of ethanol and add water to make up to 10 ml; then add 1 ml of 2,4-dinitrophenylhydrazine solution into 1 ml of this solution, and, after treatment similar to above-mentioned, let it stand for 5 min. The color in the test sample solution shall not be darker than the yellowish-red shown in the standard solution.
    8. Fusel oil (as C5H12O) Dissolve 1 g of sample in water to make 10 ml solution. Take 1 ml of this solution, and gently add 2 ml of freshly prepared vanillin-sulfuric acid solution (0.5 g vanillin in 100 ml sulfuric acid), followed by stirring. After heating for 15 min in boiling water, add 1 ml of water and, after sufficient stirring, let it stand for 15 min. Compare this color with the color obtained as follows: Mix 0.6 ml of water with 0.4 ml of isoamyl alcohol standard solution (0.01 mg C5H12O/ml), and gently add 2 ml of vanillin-sulfuric acid solution; after treatment similar to the above-mentioned, let it stand for 15 min. The color in the sample solution shall not be darker than the yellowish-red given in the standard solution.
    9. Methanol (CH3OH) Methanol content shall be tested in accordance with the gas-chromatography method 5.32 of JIS K 8001 under following conditions:
    9.1 Type of detector Hydrogen flame-ionization detector.
    9.2 Required sensitivity of detector Adjust the sensitivity so that the peak height of methanol in the test sample is not less than 10 % of the effective width of the recording paper.
    9.3 Analysis Conditions
    (a) Column packing The packing should be capable of   completely separating methanol and ethanol.
    (Suggested packings are PORAPAK Q, PORAPAK QS, etc.)
    (b) Column dimensions The column should be of 2 to 4 mm in bore and 2 to 3 m in length.
    (c) Temperature of column container About 130°C.
    (d) Carrier gas Nitrogen or helium, at a flow rate of about 30 ml/min.
    (e) Fuel gas Hydrogen 98 kPa (1kgf/cm2)
    (f) Ignition-improver gas Air 196 kPa (2 kgf/cm2)
    9.4 Preparation of standard sample Mix 100 g of sample with 20 mg of methanol.
    9.5 Operation Using the gas chromatograph, measure the peak area (A1) of methanol in the test sample and the peak area (A2) of the standard sample with methanol added.
    A1 should not be larger than A2 - A1.
    10. Benzene and other organic impurities Measure the absorbance of the sample standard with the wavelength of maximum absorption, in the neighborhood of 255 nm, taking water as the contrast solution, using a 10 mm quartz absorption cell, in accordance with JIS K 0115. The absorbance shall be not more than 0.11.
    11. Permanganate reducing substances Add 0.1 ml of 0.02 mol/l (0.1N) potassium permanganate solution to 20 ml of the sample that has been adjusted to 25°C, and, after agitating it, hold it for 5 min at 25°C. The color of this solution shall not be lighter than the red color given by a colorimetric standard solution.
    12. Sulfuric acid coloring substances This test shall be in accordance with method 5.26 (2) (a) of JIS K 8001. In this instance, when 10 ml of sample are mixed with 10 ml of sulfuric acid, there should be no development of color.
    13. Ethanol Content (by specific gravity) According to the value obtained in test 2, the specific gravity should be not more than 0.793.


    Reference Table Specific Gravity Table of Ethanol (99.16 to 100.01 v/v %)

    Specific gravity (20/20°C)

    		 Contents v/v %

    Specific gravity (20/20°C)

    		 Contents v/v %

    Specific gravity (20/20°C)

    		 Contents v/v %

    Specific gravity (20/20°C)

    		 Contents v/v %

    Specific gravity (20/20°C)

    		 Contents v/v %

    0.7949

    		 99.16 0.7939 99.36 0.7929 99.56 0.7919 99.77 0.7909 99.96

    8

    		 99.19 8 99.38 8 99.59 8 99.78 8 99.98

    7

    		 99.20 7 99.40 7 99.61 7 99.80 7 99.99

    6

    		 99.22 6 99.43 6 99.62 6 99.82 6 100.01
    5 99.24 5 99.44 5 99.64 5 99.83
    4 99.27 4 99.46 4 99.67 4 99.86
    3 99.28 3 99.48 3 99.69 3 99.88
    2 99.30 2 99.51 2 99.70 2 99.90
    1 99.32 1 99.53 1 99.72 1 99.91
    0 99.35 0 99.54 0 99.74 0 99.93


    5.2 GRADE 1: Test methods for this grade are the same as for Premium Grade above, with the following variations:

     

    1. Non-volatile matter The non-volatile matter shall be measured in accordance with method 5.1 (4). But, in this instance, the sample should be 50 g and the residue should be not more than 1.5 mg.
    2. Heavy metals, as Pb The heavy metals shall be measured in accordance with method 5.1 (6), with minor variations, as appropriate.

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