ASTM-D5837 Furans in Insulating Liquids PDF

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Designation:
on: D 5837 – 99 (Reap
(Reapprov
proved
ed 2005)
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Standard Test Method for

Furanic Compounds in Electrical Insulating Liquids by High-
Performance Liquid Chromatography (HPLC) 1
This standard is issued under the fixed designation D 5837; 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
cript epsilon (e) indicates an editorial change since the last revision or reapproval.
superscript
supers
1. Sco
Scope
pe 2. Referenced Documents
1.1 This test method covers the determinatio
determinationn in electrical
electrical 2.1 ASTM Standards: 2
insulating liquids of products of the degradation of cellulosic D 923 Practices for Sampling Electrical Insula
materi
mat erials
als suc
suchh as pap
paper
er,, pre
pressb
ssboar
oard,
d, and cot
cotton
ton mat
materi
erials
als D 3487 Specific
Specification
ation for Miner
Mineral
al Insu
Insulati
lating
ng
typically found as insulating materials in electrical equipment. Electrical Apparatus
These degradation products are substituted furan derivatives, D 3612 Test
Test Met
Method
hod for Analysi
Analysiss of Gas
Gaseses
commonly referred to as furanic compounds or furans. This Electrical Insulating Oil by Gas Chromatogra
test method allows either liquid/liquid or solid phase extraction D 3613 Practice
Practice for Sampling Insulating
Insulating Liqu
(SPE)
(SP E) of the furfurani
anicc com
compou
pounds
nds fro
from
m the sam
sample
ple mat
matrix
rix Analysis and Determination of Water Conten
followed by analysis for specific furanic compounds by HPLC 2.2 International Electrotechnic
Electrotechnical
al Commission
or direct injection for analysis of specific furanic compounds dard:
by HPLC. Method
Meth od 1198
1198 Furan
Furanic
ic Compounds
Compounds Analysis
Analysis in
3
1.2 The individual
individual furanic
furanic comp
compounds
ounds that may be ident
identi-
i- Insulating Oil
fied and quantified include the following:
3. Terminology
5-hydroxymethyl-2-furaldehyde
furfuryl alcohol 3.1 Definitions of Terms Specific to This Stand
2-furaldehyde
2-acetylfuran
3.1.1 adsorbent , n—th
—thee sta statio
tionar
nary
y pha
phase
se
5-methyl-2-furaldehyde extraction; silica is used as the adsorbent in this t
3.1.2 extract , n—the liquid phase of a liquid/li
1.3 The direct injection
injection method generally has a higher
higher limit
tion containing the compound that has been extrac
of detection, especially for furfuryl alcohol. Greater interfer-
will be analyzed.
encee for furfuryl
enc furfuryl alc
alcoho
oholl may be exp expect
ected
ed whe
whenn usi
using
ng the
3.1.3 liquid/liquid
liquid/liquid extraction, n—th —thee pre
prepar
par
direct injection method as opposed to extraction methods.
extraction by mixing nonpolar test specimen with p
1.4 This test method
method has been used to successfully
successfully test for
to preferentially partition and concentrate polar co
furanic
furan ic compo
compounds
unds in mine
mineral
ral insu
insulati
lating
ng oil, sili
silicone
cone fluid,

interest from an insulating liquid test specimen.
high
hig h fire poi
point
nt ele
electr
ctrica
icall ins
insula
ulatin
ting
g oil
oilss of min
minera
erall ori
origin
gin,, Sign upphase
3.1.4 mobile to vote
, non
—thethiscarrier
title liquid phase
askarels, and perchloroethylene-based dielectric fluids.
1.5
1.5 Th
Thee va
valu
lues
es st
stat
ated
ed in SI un unit
itss ar
aree to be re
rega
gard
rded
ed as
system
analytical Usefulused toNot useful
transfer the prepared test
and through the analytical column and detector; t
standard. No other units of measurement are included in this
tion of the mobile phase affects elution time and s
standard.
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solid-phase extraction cartridge, followed by solvent elution ment to displace atmospheric gases dissolved in
from the extraction cartridge. phase solvents and to prevent the evolution of air
 Sheet Music 3.1.6 ultraviolet (UV) , adj—referring to that region of the 7.4 The analytical apparatus may be heated sev
electromagnetic spectrum including wavelengths from 10 to Celsius above ambient if necessary to reduce
380 nm. The UV detectors of most HPLC systems operate in analytical results that may be caused by tempera
the range of wavelengths from 190 to 380 nm. tions. Operation at ambient temperature or
temperature of 30 to 40°C has been found satisfact
4. Summary of Test Method laboratories.
4.1 Furanic compounds in electrical insulating liquids are 7.5 The following range of HPLC analytical co
extracted from a known volume of test specimen by means of been found to be satisfactory for extracted
a liquid/liquid extraction or solid-phase extraction. A direct (specific examples are given in the appendix):
injection of the oil also may be used. Injection Volume 15 to 30 µL
Mobile Phase water/acetonitrile or water/methanol gra
4.2 A portion of the extract or an aliquot of the oil is Flow Rat e 0.5 mL/ min to 1. 5 mL/min
introduced into an HPLC system equipped with a suitable Column Temperature ambient to 40°C
analytical column and UV detector. Column 3.9 3 300 mm C18 60 to 125A, 4 to 10 µ
mm PRP-1 100 A, 5 to 10 µm
4.3 Furanic compounds in the test specimen are identified Gradient see appendix
and quantified by comparison to standards of known concen-
NOTE 1—Some laboratories have found it beneficial to
tration.
phase solvents with a 0.45-µm or smaller polytetrafluoroet
filter. Store water in containers shielded from light. Some l
5. Significance and Use 50 mL of methanol added to 4 L of water to inhibit biolo
5.1 Furanic compounds are generated by the degradation of 7.6 The following HPLC analytical condition
cellulosic materials used in the solid insulation systems of found to be satisfactory for direct injection of the
electrical equipment.
Inject ion volume 20 to 30 µL
5.2 Furanic compounds which are oil soluble to an appre- Mobile phase acetonitrile/water gradient
ciable degree will migrate into the insulating liquid. Flow rate, initial 0.5–1.0 mL/min
Column temperature ambient to 30°C
5.3 High concentrations or unusual increases in the concen-
You're ReadingColumn a Preview Waters Nova-Pak C18 Reversed Pha
T
trations of furanic compounds in oil may indicate cellulose mm, 60A, 4 µm
degradation from aging or incipient fault conditions. Testing Gradient see Appendix
Unlock full access with a free trial.
for furanic compounds may be used to complement dissolved 7.7 For direct injection, a fixed wavelengt
gas in oil analysis as performed in accordance with Test and 281 nm has been found to provide the best chro
Method D 3612. Download WithforFree Trial
all compounds of interest, except furfuryl alcoh
best measured with a separate test using a wavelen
6. Interferences 215 and 220 nm. Each furanic compound has a ch
6.1 Materials used in the manufacture of the polypropylene maximum light absorbance occurring within
tubes and polyethylene frits of some commercially prepared ranges of wavelengths. Use of variable wavelen
solid-phase extraction columns may interfere with the deter- array detectors allows the selection of a specific wa
mination of furanic compounds, such as furfuryl alcohol and each furanic compound. Each laboratory  sha
5-hydroxymethyl-2-furaldehyde. Sign up to vote on this title
specific wavelength to yield maximum absorban
6.2 The use of acetone in any preparative or analytical step  as
compound Useful
follows: Not useful
will cause accelerated sample decay and may interfere with the Furanic Compound
accurate determination of 5-hydroxymethyl-2- furaldehyde. 5-hydroxymethyl-2-furaldehyde
furfuryl alcohol
6.3 The use of cellulosic filtering media may serve to adsorb
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8.6 Hexane—HPLC grade. mobile phase. The resulting concentration is
8.7 5-Hydroxymethyl-2-Furaldehyde —99 % purity, CAS µg/L) for each of the five furanic compou
 Sheet Music #67-47-0. indicated in 10.1.1.
8.8 Methanol—HPLC grade.
8.9 5-Methyl-2-furaldehyde —99 % purity, CAS #620-02-0. 11. Preparation of Calibration Standards in
8.10 Silica SPE Column—Solid-phase extraction column 11.1 Prepare standards of furanic compounds in
filled with 500 mg of silica. tric liquid which has been tested and shown
8.11 Toluene—HPLC grade. baseline for the range of retention times for the co
8.12 Vacuum Manifold —Device to pull vacuum on solid- interest. Mineral oil shall otherwise conform to S
phase extraction column in order to pass sample and eluent D 3487. Other dielectric liquids should confo
through SPE column. cable ASTM specifications.
8.13 Volumetric Test Tube—Test tube designed to volu-
NOTE 2—The same type of dielectric liquid should be
metrically measure in 0.10-mL graduations. preparation as the dielectric liquid found in the test specim
8.14 Vortex Mixer . method has been developed for mineral oil, but has be
8.15 Water —HPLC grade. applicable to other dielectric fluids.
11.2 Volumetric Preparation :

9. Sampling 11.2.1 Use a graduated 1-µL syringe to inject vo
9.1 Obtain test specimens (insulating fluid samples) in five furanic compounds as listed in 10.1.2 into 8 m
accordance with the procedures for sampling in Practices Dissolve the compounds and add quantitative
D 923 or Practice D 3613. volumetric flask. Make sure all compounds are
mixed.
10. Preparation of Extraction Standards in Solvent 11.2.2 Dilute the 8 mL of toluene containing f
10.1 Prepare the extraction standards by dilution of a pounds to a total volume of 1 L with electrical insu
weighed standard compound to a standard volume or by mineral origin. The solution yields a concentratio
volumetric addition of a standard compound to a standard (1000 µg/L) of each of the five furanic compoun
You're
volume in accordance with either of the procedures described Reading a Preview
described in 10.1.1.
in 10.1.1 or 10.1.2. 11.3 Gravimetric Preparation :
Unlock full access with11.3.1
a free trial.
Weigh out 0.100 g 6 5 % of each of the
10.1.1 Weight Procedure —Weigh out 0.100 g 6 5 % of
each of the five furanic compounds listed in this test method compounds and record the weight to the ne
Dissolve the weighed portion in toluene and dilut
and record the weight to the nearest 0.1 mg. DissolveDownload
weighed With Free Trial
portions into 100 mL of acetonitrile or methanol. Take 1 mL of cally to 100 mL in toluene. Mix thoroughly so
this solution and add to a clean 1-L volumetric flask. Add 199 furanic compounds are dissolved completely.
mL of either acetonitrile or methanol, using the same solvent as 11.3.2 Volumetrically dilute 1 mL of the tolu
was used earlier to dissolve the weighed portions of the furanic from 11.3.1 to 1 L using electrical insulating oi
compounds. Bring the solution in the volumetric flask to 1 L origin. This solution of furanic compounds
with water. Other ratios of solvent to water may be used such concentration of about 1 mg/L (1000 µg/L)
furanic compounds. Use 
as to match that of the initial mobile phase. This solution yields Sign up to vote onthe
thisactual
title mass of each
a concentration of about 1 mg/L (1000 µg/L) of each of the recorded in 11.3.1 to calculate the exact concent
furanic compounds. Use the actual mass of each compound to resulting solution.  Not
Useful Store useful in 10.1.1
as described
calculate the concentration. Store in a clean, dark plastic
container. Do not store in glass. 12. Liquid/Liquid Extraction Procedure—Met
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Legend:
A. 5-hydroxymethyl-2-furaldehyde
B. 2-furfuraldehyde
C. 5-methyl-2-furaldehyde
D. 2-acetylfuran
E. furfuryl alcohol
FIG. 1 Example of a Calibration Curve
You're Reading a Preview
pass the extract through a precolumn.4 If a precolumn is used, the 14. Calibration
laboratory needs to verify by experimentation that there is no significant
loss of furanic compounds. 14.1 Calibration consists of development of
curve for each furanic compound, development o
13. Solid Phase Extraction (SPE)—Method B Download With Free Trialfor each extracted furanic compo
efficiencies
13.1 Insert SPE column(s) into the vacuum manifold and single-point calibration of equipment. Determinati
pass 3 to 5 mL of hexane through each SPE column under tion efficiencies is not necessary for the dir
vacuum. Do not dry the column. method.
13.2 Mix 10 mL of test specimen with 10 mL of hexane and 14.2 Calibration Curve :
pass through SPE column at a rate no faster than 3 mL/min. 14.2.1 As appropriate, for each furanic compou
Other quantities of oil can be used as long as it is verified that extraction standard in the solvent prepared  in acco
the extraction efficiencies are unchanged. Sign
Section 10 toup to vote on
determine thethis title time.
retention
13.3 Pass 10 to 20 mL hexane through the SPE column to
rinse out residual oil and dry the column under vacuum for 5
Develop
14.2.2 Useful a  Not useful
calibration curve for each c
three separate points representing three orders of
min. Discard all eluates.
13.4 Elute retained compounds from the SPE column using such as 10 µg/L, 100 µg/L, and 1 mg/L (1000
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TABLE 1 Typical Extraction Efficiencies the same aliquot volume (10 mL for extracted sam
Liquid/Liquid Solid-Phase unknown test specimen as that which is used for th
 Sheet Music
5-hydroxymethyl-2-furaldehyde
Extraction, %
97–100
Extraction, %
97–100
standard.
furfuryl alcohol 76–83 95–100 16. Calculation

2-furaldehyde 71–77 88–96
2-acetylfuran 66–72 89–97
16.1 Identify the furanic compounds repres
5-methyl-2-furaldehyde 63–68 93–99 individual peak by comparison of retention time
obtained for the standards during the calibration p
16.2 Determine the integrated peak area for eac
of interest.
compound is used to calculate the extraction efficiency from 16.3 Calculate the concentration of each furani
the appropriate equation as follows: using the following equation:
For liquid/liquid extraction: C T 5 ~ RT / RS ! 3 C S 3 ~ V T / V E
!
EE , % 5 ~ Ro / Rs! 3 ~ V E /10! 3 D f 3 100 (1)
where:
For solid-phase extraction: C T = concentration of furanic compound of in
EE , % 5 ~ Ro / Rs! 3 ~ V E /10! 3 100 (2) test specimen,
RT = integrated peak area for the furanic co
interest in the test specimen,
where: RS = integrated peak area for the furanic co
EE = extraction efficiency calculated and expressed as a interest in the daily calibration standard
percentage, C S = concentration of the furanic compound o
Ro = average integrated peak area of calibration standard the daily calibration standard in oil
in oil at 1 mg/L (1000 µg/L), samples,
Rs = average integrated peak area of extraction standard in V E = volume of extraction solvent used
solvent at 1 mg/L (1000 µg/L), calibration standard in oil for extracted sa
V E = volume of solvent or solvent water mix You're
used Reading
for a Preview
V = volume of extraction solvent used to ext
T
extraction (generally 1 to 2.5 mL), specimen. For the direct injection techniq
10 = constant (volume of oil standard used for Unlock full access
analysis is with a freeomitted
trial. as there are no extraction vol
10 mL), and considered.
D f = dilution factor for liquid/liquid extraction. This is the
water to solvent ratio in the initial mobile Download
phase of With Free
17. Trial
Report
HPLC. If there is no dilution of the extract, D f = 1. If 17.1 Report the following information:
the extract is diluted with water before injection, 17.1.1 A reference to this test method,
D f = volume of dilution water/volume of extract. 17.1.2 Identification of the test specimen, and
14.3.2 Typical extraction efficiencies based on one labora- 17.1.3 Concentration in the test specimen of
tory’s experience are in Table 1. compound determined.
14.3.3 Determine extraction efficiencies periodically in ac- 
Sign up
18. Precision andto vote
Biason this title
cordance with 14.3.1, using the same time interval as that
followed for determination of calibration curves as indicated in 18.1  Useful 
Repeatability : Not useful
14.2.4. 18.1.1 An estimate of repeatability by standard
liquid/liquid extraction of furanic compounds in m
14.3.4 On a daily basis, run a single extraction standard in
be fo d by labo be fo
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95 % repeatability interval as % of mean (nominal concentration of 100 µg/ 2-furaldehyde: 10.6 %
kg): 2-acetylfuran: 12.6 %
5-hydroxymethyl-2-furaldehyde: 5.5 %

5-methyl-2-furaldehyde: 6.0 %
Sheet Music furfuryl alcohol: 16.7 % 95 % repeatability interval as % of mean (nominal concentration
2-furaldehyde: 6.0 % kg):
2-acetylfuran: 7.7 % 5-hydroxymethyl-2-furaldehyde: 3.9 %
5-methyl-2-furaldehyde: 6.0 % 2-furaldehyde: 3.7 %
95 % repeatability interval as % of mean (nominal concentration of 1000 µg/ 2-acetylfuran: 3.2 %
kg): 5-methyl-2-furaldehyde: 2.1 %
5-hydroxymethyl-2-furaldehyde: 10.2 %
furfuryl alcohol: 13.7 % 18.2 Reproducibility —A round-robin is planned
2-furaldehyde: 9.6 % reproducibility of this test method.
2-acetylfuran: 11.0 %
18.3 Bias—A round-robin is planned to establi
5-methyl-2-furaldehyde: 11.0 %
test method.
18.1.3 An estimate for repeatability by standard deviation
for the direct injection method of furanic compounds in 19. Keywords
mineral oil has been found by one laboratory to be as follows 19.1 direct injection; furaldehyde; furanic; fura
for ten replicates: furfural; furfuraldehyde; furfuryl alcohol; furfuryl
95 % repeatability interval as % of mean (nominal concentration of 100 µg/ ryl; HPLC; liquid/liquid extraction; solid-pha
kg): SPE; 5-hydroxymethyl-2-furaldehyde;
5-hydroxymethyl-2-furaldehyde: 4.9 % 2-acetylfuran; 5-methyl-2-furaldehyde
APPENDIXES
(Nonmandatory Information)
X1. EXAMPLE CHROMATOGRAMS
Download With Free Trial
Retention Time, min Compound

2.91 5-hydroxymethyl-2-furaldehyde
3.65 furfuryl alcohol 
4.32 2-furaldehyde Sign up to vote on this title
5.27
6.42
2-acetylfuran
5-methyl-2-furaldehyde  Useful
Retention Time, min
2.22  Not useful Compound
5-hydroxymethyl-2-fu
Extraction: Solid phase extraction (SPE) 4.11 furfuryl alcohol
Column temperature: 30°C 5.86 2-furaldehyde
I j ti l 15 L 8 71 2 acetylfuran
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ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
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This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.
This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM websit
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ASTM-D5837 Furans in Insulating Liquids PDF

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ASTM-D5837 Furans in insulating

    18678589- hplc ASTM-

Standard Test Method for

ASTM-D5837 Furans in insulating

    18678589- hplc ASTM-

ASTM-D5837 Furans in insulating

    18678589- hplc ASTM-

11.2 Volumetric Preparation :

ASTM-D5837 Furans in insulating

    18678589- hplc ASTM-

ASTM-D5837 Furans in insulating

    18678589- hplc ASTM-

furfuryl alcohol 76–83 95–100 16. Calculation

ASTM-D5837 Furans in insulating

    18678589- hplc ASTM-

X1. EXAMPLE CHROMATOGRAMS

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Retention Time, min Compound

ASTM-D5837 Furans in insulating

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ASTM-D5837 Furans in insulating

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