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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.
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.
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.
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.
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.
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.
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
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
)
Group 2 )
96
)
Group 3 )
Hi-flash solvent
Heavy solvent naphtha
78
Standing Time
min.
15