Designation: D 2668 – 02
Standard Test Method for
2,6-di-tert-Butyl-p-Cresol and 2,6-di-tert-Butyl Phenol in Electrical
Insulating Oil by Infrared Absorption 1
This standard is issued under the fixed designation D 2668; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope * 3.3 When making this test on other than a highly oxidized
1.1 This test method covers the determination of the weight oil or when using a double-beam spectrophotometer, it has
percent of 2,6-ditertiary-butyl paracresol and 2,6-ditertiary- been found convenient to obtain the spectrum between 2.5 µm
butyl phenol in new or used electrical insulating oil in (4000 cm−1) and 2.9 µm (3450 cm−1) because the instrument is
concentrations up to 0.5 % by measuring its absorbance at the compensated for the presence of moisture and the band is not
specified wavelengths in the infrared spectrum. influenced by intermolecular forces (associations). However,
1.2 This standard does not purport to address all of the when testing a highly oxidized oil or when using a single-beam
safety concerns, if any, associated with its use. It is the instrument better results may be obtained if the scan is made
responsibility of the user of this standard to establish appro- between 10.90 µm (918 cm−1) and 14.00 µm (714 cm−1).
priate safety and health practices and determine the applica- 3.4 Increased absorption at 11.63 µm (860 cm−1) or 13.33
bility of regulatory limitations prior to use. µm (750 cm−1) or both, will identify the inhibitor as 2,6-
ditertiary-butyl paracresol or 2,6-ditertiary-butyl phenol re-
2. Referenced Documents spectively (Note 1).
2.1 ASTM Standards: NOTE 1—The absorbance at 750 cm−1 for 2,6-ditertiary-butyl phenol
D 923 Test Method for Sampling Electrical Insulating and at 860 cm−1 for 2,6-ditertiary-butyl paracresol for equal concentra-
Liquids 2 tions will be in the approximate ratio of 2.6 to 1.
D 2144 Test Methods for Examination of Electrical Insu-
lating Oils by Infrared Absorption 2 4. Apparatus
D 3487 Specification for Mineral-Insulating Oil Used in 4.1 With equipment description referring to compliance, the
Electrical Apparatus 2 equipment shall be in accordance with Section 6 of Test
Methods D 2144. Accordingly, the use of Fourier-transform
3. Significance and Use rapid scan infrared spectrophotometers is permitted by refer-
3.1 The quantitative determination of 2,6-ditertiary-butyl ence to that test method.
paracresol and 2,6-ditertiary-butyl phenol in a new electrical
insulating oil measures the amount of this material that has 5. Sampling
been added to the oil as protection against oxidation. In a used 5.1 Obtain the sample in accordance with Test Method
oil it measures the amount remaining after oxidation products D 923.
have reduced its concentration. The test is also suitable for
manufacturing control and specification acceptance. 6. Calibration and Standardization
3.2 When an infrared spectrum is obtained of an electrical 6.1 When the manufacturer of the oil is known and the base
insulating oil inhibited with either of these compounds there is oil is available, use it to prepare the standards. For oils of
an increase in absorbance of the spectrum at several wave- unknown origin, use base oils which meet the requirements of
lengths (or wavenumbers). 2,6 ditertiary-butyl paracresol pro- Specification D 3487. Some base oils may provide a better
duces pronounced increases in absorbance at 2.72 µm (3680 match than others and therefore it is desirable to have several
cm−1), and 11.63 µm (860 cm−1). 2,6 ditertiary-butyl phenol available.
produces pronounced increases in absorbance at 2.72 µm (3680 6.2 Prepare standards containing between 0.05 and 0.4
cm−1) and 13.33 µm (750 cm−1). weight percent of 2,6-ditertiary-butyl paracresol or 2,6-
ditertiary-butyl phenol dissolved in an uninhibited base oil.
Obtain a spectrum, at the desired band, of each standard in
1
This test method is under the jurisdiction of ASTM Committee D27 on accordance with Test Methods D 2144. Cells with a standard
Electrical Insulating Liquids and Gases and is the direct responsibility of Subcom-
mittee D27.03 on Analytical Tests. path length of 0.3 to 1.0 mm are recommended. Other path
Current edition approved Oct. 10, 2002. Published December 2002. Originally lengths may be found more suitable for different instruments or
published as D 2668 – 67. Last previous edition D 2668 – 96.
2
particular wave lengths. Other sample path lengths may be
Annual Book of ASTM Standards, Vol 10.03.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
D 2668 – 02
used provided the instrument sensitivity can be adjusted to will be necessary for determining the intensity measurements. Alterna-
compensate for this change. The dip in the curve for the tively, instrument software capable of recording all settings of the
inhibited oil should provide a distinctive increase in the spectrophotometer used in obtaining the respective spectra, may be used.
absorbance at the critical wavelength or frequency (Note 3). 6.3 The quantitative determination is made from the follow-
Repeat the procedure on each of the standards making at least ing equation which is derived from Beer’s law:
three scans on each standard. (See Note 2) Record all settings Absorbance 5 A 2 Ao
of the spectrophotometer used in obtaining the respective
spectra (Note 4). where:
Ao = absorbance units of base oil, and
NOTE 2—The current method precision is based on manually deter-
A = absorbance units of oil containing 2,6-ditertiary-butyl
mined results where exactly three scans were determined for each
standard. Newer instruments are capable of automatically performing paracresol or 2,6-ditertiary-butyl phenol.
scans much more rapidly, which can reduce the variability of results 6.4 Manual Plotting Routine for Generating Calibration
determined. In such cases, it is recommended that the number of scans be Curve—Designate the point of maximum absorbance of the
increased to statistically compensate for any outliers. Labs will need to absorbance band as Point A. Draw a tangent to the spectrum
determine the minimum number of scans that should be used in their curve and a second line through Point A perpendicular to the
instrument standardization and test specimen analyses to satisfy their absorbance lines, as shown in Fig. 1. Designate the intersection
testing needs.
NOTE 3—Where desired, a chart having a non-linear wavelength scale
of these two lines as Point Ao. Read the values of absorbance
as the abscissa may be used. at these points on the charts of the three scans made on each
NOTE 4—In making these tests, transmission-scaled charts may be test specimen to the nearest 0.001 absorbance unit (with the aid
used, but in this case special rulers and nomographs or logarithmic tables of a reading glass) and subtract the values of Ao from those of
FIG. 1 Spectrum of an Electrical Insulating Oil Inhibited with 2,6-Ditertiary-Butyl
Paracresol Showing Location Points Ao and A
2
D 2668 – 02
A. When the average of the three values for each of the calibration curve. For the Differential Method, fill the reference
specially prepared test specimens is plotted against the con- cell with an appropriate base oil free of oxidation inhibitors.
centration, a straight line is obtained. The best straight line Use a spectrophotometer which meets the requirements speci-
through the calibration data points should be drawn or deter- fied in Section 6 of Test Methods D 2144 and instrumental
mined by linear regression analysis. This is the calibration conditions identical to those used in obtaining the spectra for
curve from which the unknown concentration of the 2,6- the calibration curve.
ditertiary-butyl paracresol or 2,6-ditertiary-butyl phenol in a 7.2 For routine tests, a single scan of the test specimen is
test specimen may be determined. One such calibration curve adequate as long as the instrument is capable of meeting the
is shown as Fig. 2. Fig. 3 and Fig. 4 illustrate sections of criteria of 8.2 using single scans to replace average values. For
differential scans. referee purposes, use the average of three scans of the test
6.4.1 Automatic Plotting Routine for Generating Calibra- specimen performed manually or the average of the same
tion Curve—For instruments capable of automatically gener- number of scans used to standardize the instrument for the test
ating a standard calibration curve, follow manufacturer’s specimen, if performed automatically.
instructions. Perform at least three scans for each standard 7.3 Manually Determined Results—Read the values of ab-
analyzed across the calibration range of interest (see Note 2). sorbance at points Ao and A on each of the three spectra to the
Develop a calibration curve which has a minimum correlation nearest 0.001 absorbance unit; obtain the differences and
value of 0.99 to ensure the linearity of the calibration curve. average them. Using this average value, determine the concen-
6.5 When frequent determinations are made on a routine tration from the calibration curve.
basis, periodic checks of one or more standards are recom- 7.4 Automatically Determined Results—Using the average
mended, since the characteristics of electronics components in value of the absorbance difference between A and Ao that is
spectrophotometers change with time. If the absorbance of the determined automatically by the instrument for the same
standards differ from the calibration curve by more than the number of scans performed on the test specimen as for the
limits given in 8.2, a new curve should be obtained. Some standards, determine the concentration of the test specimen
laboratories have developed tighter limits than these. A new from the calibration curve.
curve should also be obtained whenever there is a change in
operating conditions, such as a change in light source, scan 8. Precision and Bias
speed, and so forth. 8.1 Checking Limits of Range (A − Ao)—Determine the
highest and lowest values of A − Ao resulting from the three or
NOTE 5—It is recommended that the solutions of known concentration
be stored in amber-colored bottles for a period not to exceed one year in more scans and subtract one from the other. If the resulting
order to facilitate a quick check of the characteristics of the spectropho- quantity exceeds 0.010, reject the results as excessively vari-
tometer in relation to the calibration curve. able and repeat the test.
8.2 Repeatability—The difference between two determina-
7. Procedure tions for DBPC and DBP, each obtained from the average of
7.1 Using the quantitative scan mode, make at least three three scans determined manually, obtained by the same opera-
scans (see Note 2) of the test specimen on which the determi- tor with the same apparatus under constant operating condi-
nation of the 2,6-ditertiary-butyl paracresol or 2,6-ditertiary- tions on identical test material would, in the long run, in the
butyl phenol content is to be made, at the desired band. Do this normal and correct operation of the test method, exceed the
in accordance with Test Methods D 2144, except that cells value of 0.04 % by only one case in twenty.
having path lengths as specified in 6.2 are preferred. Use the 8.3 Reproducibility—The difference between two determi-
same cell that was used in obtaining the spectra for the nations for DBPC and DBP, each obtained from the average of
FIG. 2 Calibration Curve for Determining the Percent by Weight of 2,6-Ditertiary-Butyl
Paracresol in Electrical Insulating Oil
3
D 2668 – 02
FIG. 3 Section of Differential Scan-A
FIG. 4 Section of Differential Scan-B
three scans determined manually, obtained by different opera- 9. Keywords
tors in different laboratories on identical test material would, in
9.1 2,6-ditertiary-butyl paracresol; 2,6-ditertiary-butyl phe-
the long run, in the normal and correct operation of the test
nol; electrical insulating oil; infrared absorption; paracresol
method, exceed the value of 0.04 % by only one case in twenty.
8.4 No statement is made about bias of this test method for
measuring ditertiary-butyl paracresol or ditertiary-butyl phenol
as it has not been determined.
4
D 2668 – 02
SUMMARY OF CHANGES
Committee D27 has identified the location of selected changes to this standard since the last issue (D 2668–96)
that may impact the use of this standard.
(1) Added a sentence to section 4.1 permitting use of FTIR (3) Added a new Note 2 and renumbered subsequent Notes
instruments. accordingly. Updated initial Note 3 to Note 4 and added a
(2) Updated sections 6.2, 6.4, 7.1, 7.2, 7.3, 8.1, 8.2, and 8.3. second sentence.
Added a new section 6.4.1 and 7.4.
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