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1. Scope
1.1 This test method covers three procedures for the determination of total sulfur in petroleum products including
lubricating oils containing additives, and in additive concentrates. This test method is applicable to samples boiling above
177C (350F) and containing not less than 0.06 mass % sulfur.
Two of the three procedures use iodate detection; one employing an induction furnace for pyrolysis, the other a resistance
furnace. The third procedure uses IR detection following
pyrolysis in a resistance furnace.
1.2 Petroleum coke containing up to 8 mass % sulfur can be
analyzed.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D 1193 Specification for Reagent Water2
D 1266 Test Method for Sulfur in Petroleum Products
(Lamp Method)3
D 4057 Practice for Manual Sampling of Petroleum and
Petroleum Products4
D 6299 Practice for Applying Statistical Quality Assurance
Techniques to Evaluate Analytical Measurement System
Performance5
6. Apparatus
6.1 Combustion and Iodate Detection System
6.1.1 FurnacesTwo major types are available, the primary difference being the manner in which the necessary high
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D 1552
dependent on the type of furnace used and is available from the
manufacturer of the specific combustion unit. To attain the
lower sulfur concentration given in Section 1, the ceramics
used with the induction furnace assembly shall be ignited in a
muffle furnace at 1371C (2500F) for at least 4 h before use.
6.4 Sieve, 60-mesh (250-mm).
6
The Models SC32, or SC132, manufactured by LECO Corp., 3800 Lakeview
Ave., St. Joseph, MI 49085-2396, have been found satisfactory for this purpose.
7
Reagent Chemicals, American Chemical Society Specifications, Am. Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals,
BDH Ltd., Poole, Dorset, U. K. and the United States Pharmacopeia and National
Formulary, U. S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D 1552
TABLE 1 Sample Weight for Induction Furnace
Sulfur Content, %
Weight of Sample
to be Taken, mg
90A
50 to 90
50 to 90
12.1.1
0 to 2
2 to 4
4 to 10
Over 10
A
8. Sampling
8.1 Take samples in accordance with the instructions in
Practice D 4057.
9. Preparation of Apparatus
9.1 Induction-Type FurnaceAssemble the apparatus according to the instructions furnished by the manufacturer.
Purify the oxygen by passing it through (1) H2SO4 (relative
density 1.84), (2) Ascarite, and (3) magnesium perchlorate
(Mg(ClO4)2) or phosphorus pentoxide (P2O5) (Warningsee
7.4). Connect a rotameter between the purifying train and the
furnace. Insert a small glass-wool plug in the upper end of the
glass tubing connecting the furnace with the absorber to catch
oxides of tin. Connect the exit end of the combustion tube to
the absorber with glass tubing, using gum rubber tubing to
make connections. Position the absorber so as to make this
delivery line as short as possible. Fig. 2 illustrates schematically the assembled apparatus. Adjust the oxygen flow to 1 6
0.05 L/min. Add 65 mL of HCl (3 + 197) and 2 mL of
starch-iodide solution to the absorber. Add a sufficient amount
of the appropriate standard KIO3 solution (Table 1) to produce
a faint blue color. This color will serve as the end point for the
titration. Adjust the buret to zero. Turn on the furnace filament
switch and allow at least 1 min warm-up before running
samples (Warningsee 7.4).
9.2 ResistanceType FurnaceAssemble the apparatus according to the instructions furnished by the manufacturer.
Purify the oxygen by passing it through (1) H2SO4 (relative
density 1.84), (2) Ascarite, and (3) Mg(ClO4)2 or P2O5
(Warningsee 7.4). Connect a rotameter between the purifying train and the furnace. Fig. 3 illustrates schematically the
assembled apparatus. Turn on the current and adjust the
furnace control to maintain a constant temperature of 13166
14C (2400 6 25F). Adjust the oxygen flow rate to 2 6 0.1
L/min. Add 65 mL of HCl (3 6 197) and 2 mL of starch-iodide
solution to the absorber. Add a few drops of the appropriate
standard KIO3 solution (Table 2) to produce a faint blue color.
Adjust the buret to zero.
9.3 ResistanceType FurnaceIR DetectionAssemble and
adjust apparatus according to manufacturers instructions.
Initialize microprocessor, check power supplies, set oxygen
pressure and flows and set furnace temperature to 1371C
(2500F).
Normality of Standard
KIO3 solution for Titration
0.006238
0.006238
0.01248
(Note 2)
Approximate.
Weight of Sample
to be Taken, mg
0 to 2
2 to 5
5 to 10
Over 10
100 to 200
100 to 200
100 to 200
(Note 2)
Normality of Standard
KIO3 solution for Titration
0.006238
0.01248
0.06238
(Note 2)
where:
SA = mass percent sulfur in potassium alum used,
WA = milligrams of potassium alum used,
(1)
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crucible. Make a depression in the bed with the end of a stirring
rod. Weigh the crucible to 0.1 mg. Weigh into the depression
the proper amount of sample according to Table 1 (12.1.1)
(Note 2). Cover the sample with a separator disk (Note 3).
Place on the separator disk the predetermined amount of iron
chips necessary to obtain the required temperature (6.1.1.2).
This is usually between 1.2 and 2.0 g, but should be held
constant with 60.05 g. Sprinkle about 0.1 g of tin on the iron.
Cover the crucible with a lid and place on the furnace pedestal.
12.1.1 Under no conditions shall an organic sample larger
than 100 mg be burned in an induction-type furnace.
Va
(2)
where:
Ss = mass percent sulfur in standardization sample used,
Ws = milligrams of standardization sample used,
Vb = millilitres of standard KIO3 solution used in the blank
determination,
Vs = millilitres of standard KIO3 solution used in determining the standardization factor, and
C = sulfur equivalent of the standard KIO3 solution used
in determining the standardization factor, mg/mL.
10.1.3 Quality ControlRun a suitable analytical quality
control sample several times daily. When the observed value
lies between acceptable limits on a quality control chart,
proceed with sample determinations.
D 1552
17. Quality Control
17.1 Confirm the performance of the test procedure by
analyzing a quality control sample that is stable and representative of the sample of interest.
17.1.1 When the quality control/quality assurance protocols
are already established in the testing facility, these may be used
to confirm the reliability of the test result.
17.1.2 When there is no quality control/quality assurance
protocol established in the testing facility, Appendix X1 can be
used for this purpose.
IR8
0.04
0.07
0.09
0.12
0.13
0.16
15. Calculation
15.1 Calculation for Iodate DetectionCalculate the sulfur
content of the sample as follows:
Sulfur, mass % 5 ~100 ~V 2 Vb! 3 Fs 3 C!/W
Repeatability
Iodate
0.05
0.07
0.10
0.16
0.22
0.24
Reproducibility
Iodate
0.08
0.11
0.17
0.26
0.40
0.54
IR8
0.13
0.21
0.27
0.38
0.44
0.49
(3)
where:
V = standard KIO3 solution, mL, used in the analysis,
Vb = standard KIO3 solution, mL, used in the blank determination,
Fs = standardization factor (see 10.1.2),
C = sulfur equivalent of the standard KIO3 solution used
in the analysis, mg/mL, and
W = milligrams of sample used in the analysis.
15.2 Calculation for IR Detection:
15.2.1 Report all results using the microprocessor.
15.2.2 Report the average of two results.
r 5 0.05X
(4)
16. Report
16.1 In the range from 0.05 to 5.00 mass % sulfur, report to
the nearest 0.01 mass %. In the range from 5 to 30 mass %
sulfur, report to the nearest 0.1 mass %.
5
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R 5 0.22X
(5)
19. Keywords
APPENDIX
(Nonmandatory Information)
X1. QUALITY CONTROL
10
ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis, 6th
ed., available from ASTM Headquarters.
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