STANDARD TEST FOR WATER MISCIBILITY OF WATER-SOLUBLE SOLVENTS

ASTM D 1722 90
Scope:
This test method covers the determination of the miscibility of water-soluble solvents with water.
While written specifically for testing acetone, isopropyl alcohol (isopropanol) and methyl alcohol
(methanol), the method is suitable for most water-soluble solvents.
This method serves to detect water immiscible contaminants qualitatively; the level of detection of
these impurities varies widely with both the type of solvent and the type of impurity.
The level of detection of water-insoluble materials depend upon the solvent tested and the type of
impurity or impurities present. That is paraffin, olefin, aromatic, high molecular weight alcohol, or
ketone, etc. There is, therefore, no specific level of impurity detected by this procedure.
This test is normally performed at ambient temperatures.
Summary of Method:
The specimen is diluted to 10 volumes with water and the resulting mixture examined for cloudiness or
turbidity.
Significance and use:
Water-insoluble materials present in a solvent expected to be completely water miscible may interfere
with many uses of the solvent. This test method provides a measure of the miscibility of water-soluble
solvents with a polar medium water. It also provides a qualitative indication of the presence of waterimmiscible contaminants.
The results of this test method may be used in assessing compliance with a specification. Prior to
agreeing to this test method as the basis of a specification requirement, it may be desirable that the
interpretation of what constitutes cloudiness or turbidity be agreed upon between the supplier and the
purchaser.
Apparatus:
Cylinder, graduated, glass-stoppered, 250 ml
Reagent:
Water References to water shall be understood to mean reagent water conforming to Type IV of
Specification D 1193.
Procedure:
Transfer 25 ml of the sample to one of two glass 250-mL graduated cylinders, dilute to the mark with
water and mix thoroughly. Allow any bubbles to rise to the surface.
Add 250 ml of water to the second cylinder and reserve as a blank.
Compare the specimen solution with the water blank by viewing through the length of the column of
liquid toward a dark background. When an artificial light source is used, position the light so that it
passes transversely through the cylinders.
Report:
If the specimen-water mixture is as free of cloudiness or turbidity as the blank, report the sample as
passes test. If any cloudiness or turbidity is detected after 30 min, report as fails test.
Precision and Bias:
Because of the pass-fail nature of this test procedure, no precision or bias statement is prescribed.

STANDARD METHOD OF TEST FOR DETECTING HYDROCARBONS IN

SMA-42-60

This method of test describes a procedure for detecting the presence of hydrocarbons in methanol by
observing any cloudiness or opalescence, which occurs when the sample is diluted with, distilled water.
1.

Wall wash the tank with methanol (about 1 sq.m.) and dilute 15 ml of this sample with 45 ml of
distilled water to a 100 ml color comparison tube. Invert the tube several times to ensure complete
mixing and allow it to stand for twenty minutes at room temperature.

2.

Fill up 100 ml blank tube with 60 ml of distilled water,

3.

Compare the sample to the distilled water blank by looking down through the tube against a black
background. To pass the test, no cloudiness or opalescence shall appear at any time during the test
period.

TESTING FOR HYDROCARBONS (WATER MISCIBILITY TEST)

This test determines the miscibility of water with Methanol and is used to test for Hydrocarbons, which
are relatively insoluble in water. When methanol is diluted with water the presence of hydrocarbons in
the methanol will result in turbidity or cloudiness in the mixture. The test procedure is as follows: 1.
2.
3.
4.

Pour 25 ml of wall wash methanol sample into a clean Nessler tube.

To this add 75 ml of deionized water.
Stopper and invert tube to mix it and allow to stand for about 20 minutes.
Place the tube on a black surface, turn off lights to darken the room and shine a penlight torch
through the side of the tube while looking down through the liquid column. A wide beam flashlight
should be used and kept about six inches from the columns.

To prepare a standard solution for comparison: 1.

2.
3.
4.

Pour 25 ml of laboratory methanol into a clean Nessler tube.

To this add 75 ml of deionized water.
Stopper and invert tube to mix it and allow to stand for about 20 minutes.
Compare the standard solution to the wall wash sample. If a bluish tint is visible, there are
moderate to heavy hydrocarbons. If a whitish haze is observed, this usually indicates slight
hydrocarbons.

Factors, which could affect this test, are: -

if graduation numbers on the tubes are in blue

if the column is dirty
if the bulkhead is damp

Pls. note: It is more critical when using a penlight for this test due to the intensity of the beam. If this method is
used on a standard (25 ml of laboratory methanol and 75 ml of deionized water) solution, there may
sometimes be a faint whitish trace in this standard solution.

TESTING FOR CHLORIDES (IN CONTINUATION OF HYDROCARBON TEST)

Using the same tube in which the Water miscibility test was done (if no hydrocarbons were found): 1.
2.
3.

Add 5 drops of Silver Nitrate 10 percent solution.

Stopper and invert the tube to mix and observe if any turbidity is formed.
Compare the turbidity of the sample with the standard by looking down through the liquid against
a black background.

Comparison of the wall wash samples to a standard should be done in a darkened room by looking
down through the tubes using a wide beam flashlight held about one foot away from the sides of the
tubes.
A standard solution for varying amounts of chloride levels may be prepared from the standard 100
PPM Chloride stock solution as below: Take 1 ml of 100-PPM standard chloride stock solution and add it to 25 ml of analytical grade
methanol. To this add 75 ml of deionized water. This solution will show turbidity equivalent to 1-PPM
chloride content.
To make a higher chloride standard, increase the amount of stock solution incrementally in the mixture,
i.e., for a 2-PPM chloride solution, add 2 ml of the 100-PPM chloride stock solution to 25 ml analytical
grade methanol and 75 ml deionized water.

STANDARD METHOD OF TEST FOR DETECTING CHLORIDES

This method describes the procedure for detecting chloride ions.
1.

Measure 20 ml of distilled water into each of 3 Nessler tubes (50-ml tubes).

2.

Pipette 5 ml of the Methanol wall wash sample into one of the Nessler tubes (Tube A).

3.

Pipette 5 ml of the methanol used in the wall wash into another Nessler tube (This will be the
blank to check whether the Methanol used is contaminated) (Tube B).

4.

Pipette 0.25 ml of the Standard Chloride solution (100 PPM) into another Nessler tube (This will
be the 5 PPM Chloride standard) (Tube C).

5.

Pipette 1 ml of 20% Nitric acid and 1 ml of 0.1 Silver Nitrate solution to all three Nessler tubes.

6.

Cap all tubes and mix well by inverting several times.

7.

Allow the contents to stand for 10 minutes in the dark before comparing the sample (Tube A) with
the standard (Tube C) by viewing against a black background.
REPORTING

If the sample cloudiness (Tube A) is less than that of the 5-PPM standard (Tube C), then report as less
than 5 PPM chlorides.
Always check the blank tube (Tube B) to ensure that the Methanol used is not contaminated. It should
not have any cloudiness and must be clear and transparent.
If higher values of chlorides are required then the following volumes of the Standard Chloride solution
(100-PPM) should be added in Tube C (Step 4).
0.50 ml of Chloride Solution for 10 PPM
0.75 ml of Chloride Solution for 15 PPM
1.00 ml of Chloride Solution for 20 PPM
1.25 ml of Chloride Solution for 25 PPM
1.50 ml of Chloride Solution for 30 PPM
1.75 ml of Chloride Solution for 35 PPM
2.00 ml of Chloride Solution for 40 ppm
2.25 ml of Chloride Solution for 45 PPM
2.50 ml of Chloride Solution for 50 PPM

STANDARD TEST METHOD FOR COLOR OF CLEAR LIQUIDS

(PLATINUM COBALT SCALE)
ASTM D1209
This test method describes a procedure for the visual measurement of the color of essentially light
colored liquids.
1.

From the stock solution prepare standards in accordance with Table I by diluting the required
volumes to 100 ml with distilled water in the Nessler tube. Cap the tubes and seal the caps with
shellac or a waterproof cement if long term storage is desired (this standard would be stable for at
least a year).

2.

Wall wash the tank using the appropriate solvent (e.g. Acetone or Methanol or Para-Xylene, etc. as
applicable) and introduce 100 ml of the specimen into a Nessler tube passing the specimen through
a filter if it has any visible turbidity.

3.

Report the standard color number, which most matches the specimen. In the event the color lies
midway between two standards, report the darker of the two or otherwise report the range over
which an apparent match is obtained.
TABLE I
COLOR
STANDARD
NUMBER
1

STOCK
SOLUTION
ml
0.20

COLOR
STANDARD
NUMBER
25

STOCK
SOLUTION
ml
5.00

0.40

30

6.00

0.60

35

7.00

0.80

40

8.00

1.00

50

10.00

1.20

60

12.00

1.40

70

14.00

1.60

100

20.00

1.80

150

30.00

10

2.00

200

40.00

11

2.20

250

50.00

12

2.40

300

60.00

13

2.60

350

70.00

14

2.80

400

80.00

15

3.00

450

90.00

20

4.00

500

100.00

STANDARD TEST METHOD FOR PERMANGANATE TIME TEST

ASTM D 1363 58
Scope:
This method serves as a means of detecting in alcohols or ketones the presence of impurities that
reduce potassium permanganate.
Applicable to Methanol, ethanol, propanol, butanol, acetone, methyl ethyl ketone and methyl isobutyl
ketone.
Summary of method:
Substances reacting with potassium permanganate in neutral solutions reduce it to manganese dioxide
that colors the solution yellow. In the permanganate test the time required for the test solution to that of
a standard solution, is measured. The color of the test solution changes from pink-orange to yelloworange.
Apparatus:
Cylinders, glass stoppered, 50 ml.
Pipette, capable of delivering 2 ml of solution.
Clock or stopwatch.
Reagents:
Potassium Permanganate solution 0.1 gr. of KmnO4 per l of water
Uranyl Nitrate cobaltous chloride, standard solution.
This standard solution represents the color of the terminal point to which the sample fades in the
KmnO4 test. This solution is stable and should be kept in a 50 ml. Glass-stoppered cylinder, exactly the
same as those in which the test is run.
Procedure:
Dissolve 0.100 gr. of KmnO4 in 500 ml. of distilled water in a volumetric flask.
Clean the glass-stoppered cylinder by 10 rinsing with tap water, 5 rinsing with distilled water and 3
rinsing with sample.
Fill the cylinder with sample up to the 50-ml. mark and place it into a constant temperature bath,
maintained at 15oC for methanol or at 25oC for acetone.
When the sample has reached the bath temperature (about 5 minutes), add 2 ml of potassium
permanganate solution, using the 2-ml. pipette.
Stopper the tube, invert once to mix the contents, and return to the bath.
Determine the time from addition of the potassium permanganate till the color matches that of the
standard solution.
Protect the tube from light during this time.
When you have finished the test, clean the sample cylinder twice with tap water and fill it with
concentrated hydrochloric acid.

ACID WASH COLOR OF AROMATIC HYDROCARBONS

ASTM D 848
Scope:
This method covers the determination of the acid wash color of benzene, toluene, xylene, refined
solvent naphthas and similar aromatic hydrocarbons.
Definition:
Acid wash color: The color developed in the separated acid when a sample is agitated with sulfuric acid
under the conditions described in this method.
Apparatus:
Acid wash color standards numbered 0 to 14.
Stoppered cylinders, 30 ml.
Procedure:
Fill a dry and clean stoppered cylinder up to the 7-ml mark with sulfuric acid of the strength specified
in Table I for the type of sample to be tested. Add sufficient sample to bring the total volume to the 28ml mark. Insert the stopper, hold a finger over the stopper and give vigorous shakes with a stroke of 5
to 10 in., shaking for a total of 150 cycles over a period of 40 to 50 sec., that is at a rate of 3 to 3.75
cycles per sec.
Allow the cylinder to stand, protected from direct sunlight, for the period of time shown in Table I.
Without further delay invert the cylinder gently once or twice to obtain a uniform color in the acid
layer, and compare the color of the acid layer with those of the standards. Make the comparison against
a white background or at daylight.
Designate the color of the acid layer by the number of the nearest matching standard and add to the
number a plus or minus sign if the sample is respectively darker or lighter than the standard color.
Note:
Caution: Concentrated Sulfuric acid will cause severe burns on contact with the skin. When spilt,
Remove with plenty of water.
Remark:
It is advisable, when performing the test, to use clean plastic throwaway gloves.
TABLE I
)
)
Group 1 )
)
)

Acid Strengths and Standing times

Acid Strengths
Sample
%
Benzene, all ASTM grades
Toluene, all ASTM grades
Xylene, nitration grades
96
Xylene, 5o
Xylene, 10o

)
Group 2 )

Xylene, industrial grade

Refined solvent naphtha

96

)
Group 3 )

Hi-flash solvent
Heavy solvent naphtha

78

Standing Time
min.
15