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D1492 - 13 Standard Test Method For Bromine Index of Aromatic Hydrocarbons by Coulometric Titration PDF
D1492 - 13 Standard Test Method For Bromine Index of Aromatic Hydrocarbons by Coulometric Titration PDF
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5. Significance and Use where such specifications are available.5 Other grades may be
5.1 This test method is useful for setting specification, for used, provided it is first ascertained that the reagent is of
use as an internal quality control tool, and for use in develop- sufficiently high purity to permit its use without lessening the
ment or research work on industrial aromatic hydrocarbons and accuracy of the determination.
related materials. This test method gives a broad indication of 7.2 Purity of Water—Unless otherwise indicated, references
olefinic content. It will not differentiate between the types of to water shall be understood to mean reagent water conforming
aliphatic unsaturation. to Type IV of Specification D1193.
6. Apparatus 7.3 Electrolyte:
6.1 Amperometric-Coulometric Apparatus, automatic, suit- 7.3.1 Preparation Cell Electrolyte—To make 1 L, mix 600
able for bromine index titrations with variable generator mL of glacial acetic acid, 260 mL of absolute methanol, and
current and timer. A typical circuit diagram of suitable equip- 140 mL of KBr solution (119g/L).
ment is shown in Fig. 1.
7.4 Potassium Bromide Solution (119 g/L)—Dissolve 119 g
6.2 Syringe, 2 mL with needle and rubber cap seal. of potassium bromide (KBr) in water and dilute to 1 L.
6.3 Stirrer, magnetic.
7. Reagents 5
Reagent Chemicals, American Chemical Society Specifications, American
7.1 Purity of Reagent—Reagent grade chemicals shall be Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
used in all tests. Unless otherwise indicated, it is intended that
Chemicals, BDH, Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
all reagents shall conform to the specifications of the Commit- and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
tee on Analytical Reagents of the American Chemical Society, MD.
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8. Hazards titration time increment is 4 s or less. Note the total titration
8.1 Consult current OSHA regulations, supplier’s Material time and generation current.
Safety Data Sheets, and local regulations for all materials used 11. Calculation
in this test method.
11.1 Calculate the bromine index, B (mg-Br/100 g), as
9. Sampling follows:
9.1 Sample the material in accordance with Practice D3437. T 3 I 3 79.9
B5 (1)
965W
10. Procedure
where:
10.1 Place 125 mL of electrolyte in a clean, dry titration
T = titration time, s
cell, insert the electrodes, and begin stirring. Verify the volume
I = generation current, mA
of electrolyte is sufficient to ensure the electrodes are com- W = weight of specimen, g
pletely submerged and if necessary, increase the volume of 79.9 = MW bromine (grams/mole), and
electrolyte required. Apply the generation current in accor- 965 = Faraday’s constant (96 500 coulomb/mole)/100
dance with Table 1.
12. Report
TABLE 1 Specimen Size and Generation Current 12.1 Report the following information:
Estimated Specimen Weight, Generation 12.1.1 Report bromine index to the nearest unit.
Bromine Index g Current, mA
0 to 20 1.000 1.0 13. Precision and Bias
20 to 200 0.600 5.0
200 to 2000 0.060 5.0 13.1 Precision—A ruggedness study was performed by
analyzing three samples 20 times and one sample five times
each over the shortest practical time. The calculated repeat-
10.2 Before introducing the specimen and immediately ability is shown in Table 2.
before each determination, bring the coulometer to equilib-
rium. TABLE 2 RepeatabilityA
Conc. mg-
10.3 Draw into the syringe the amount of sample prescribed Sample Name Replicates (n) r
Br/100 g
in Table 1 corresponding to the estimated bromine index. Wipe 997.5 mg-Br/100g Std 20 1012 39.1
Toluene-Pit EPX 20 31.2 2.9
the needle with a clean cloth, attach a rubber cap seal to the Xylene-Plant Feed 20 10.7 2.3
needle, and weigh on the analytical balance. Remove the seal, Reformate-Feed 5 670 53.9
add the specimen to the electrolyte, and set the timer to zero. A
Repeatability = SD * 2.8.
Replace the seal, reweigh the syringe, and calculate the
specimen weight.
NOTE 2—If the density or specific gravity of the specimen is known 13.2 Repeatability—See Table 2.
(Test Methods D891, D3505, or D4052 can be used), the specimen can be 13.3 Reproducibility—To be determined.
added by means of a pipet or microburet and the weight calculated.
10.4 Begin titration of the specimen. As the titration 14. Quality Guidelines
proceeds, keep the generation current at the selected value. The 14.1 Refer to Guide D6809 for suggested QA/QC activities
generation of bromine will continue as long as it is consumed that can be used as a part of this test method. It is recom-
by the sample. At the end point an incremental increase in mended that the operator of this test method select and perform
bromine concentration causes the titration and timer to stop relevant QA/QC activities like the ones in Guide D6809 to help
automatically. Forty seconds after the titration has shut off, ensure the quality of data generated by this test method.
continue the titration. If the titration cuts off, immediately, the
end point has been reached and the titration may be considered 15. Keywords
complete. Otherwise, it may be necessary to continue the 15.1 aromatic hydrocarbons; bromine index; bromine-
titration in steps, waiting about 40 s between steps, until the reactive; coulometric titration; titration
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SUMMARY OF CHANGES
Committee D16 has identified the location of selected changes to this standard since the last issue
(D1492-08ε1) that may impact the use of this standard. (Approved July 15, 2013.)
(1) Deleted Section 1.5. (5) Changed Section 13.2.1 to Section 13.1.
(2) Deleted Section 7.3. (6) Changed Section 13.2.2 to Section 13.2.
(3) Changed Section 7.3.2 to Section 7.3.1. (7) Changed Section 13.2.3 to Section 13.3.
(4) Deleted Section 13.1 through 13.1.3.
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