ASTM D1552-08(2014)
(Test Method)Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)
Standard Test Method for Sulfur in Petroleum Products (High-Temperature Method)
SIGNIFICANCE AND USE
4.1 This test method provides a means of monitoring the sulfur level of various petroleum products and additives. This knowledge can be used to predict performance, handling, or processing properties. In some cases the presence of sulfur compounds is beneficial to the product and monitoring the depletion of sulfur can provide useful information. In other cases the presence of sulfur compounds is detrimental to the processing or use of the product.
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 177°C (350°F) 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 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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.
General Information
Relations
Buy Standard
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D1552 − 08(Reapproved 2014)
Standard Test Method for
Sulfur in Petroleum Products (High-Temperature Method)
This standard is issued under the fixed designation D1552; 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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope D6792 Practice for Quality System in Petroleum Products
and Lubricants Testing Laboratories
1.1 This test method covers three procedures for the deter-
mination of total sulfur in petroleum products including
3. Summary of Test Method
lubricating oils containing additives, and in additive concen-
3.1 Iodate Detection System—The sample is burned in a
trates. This test method is applicable to samples boiling above
stream of oxygen at a sufficiently high temperature to convert
177°C(350°F)andcontainingnotlessthan0.06mass %sulfur.
about 97 % of the sulfur to sulfur dioxide. A standardization
Two of the three procedures use iodate detection; one employ-
factor is employed to obtain accurate results. The combustion
ing an induction furnace for pyrolysis, the other a resistance
products are passed into an absorber containing an acid
furnace. The third procedure uses IR detection following
solution of potassium iodide and starch indicator. A faint blue
pyrolysis in a resistance furnace.
color is developed in the absorber solution by the addition of
1.2 Petroleum coke containing up to 8 mass % sulfur can be
standard potassium iodate solution. As combustion proceeds,
analyzed.
bleaching the blue color, more iodate is added. The amount of
1.3 The values stated in SI units are to be regarded as the
standard iodate consumed during the combustion is a measure
standard. The values given in parentheses are for information
of the sulfur content of the sample.
only.
3.2 IR Detection System—The sample is weighed into a
1.4 This standard does not purport to address all of the
special ceramic boat which is then placed into a combustion
safety concerns, if any, associated with its use. It is the
furnace at 1371°C (2500°F) in an oxygen atmosphere. Most
responsibility of the user of this standard to establish appro-
sulfur present is combusted to SO which is then measured
priate safety and health practices and determine the applica-
with an infrared detector after moisture and dust are removed
bility of regulatory limitations prior to use.
by traps. A microprocessor calculates the mass percent sulfur
from the sample weight, the integrated detector signal and a
2. Referenced Documents
predeterminedcalibrationfactor.Boththesampleidentification
number and mass percent sulfur are then printed out. The
2.1 ASTM Standards:
calibration factor is determined using standards approximating
D1193 Specification for Reagent Water
the material to be analyzed.
D1266 Test Method for Sulfur in Petroleum Products (Lamp
Method)
4. Significance and Use
D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
4.1 This test method provides a means of monitoring the
D6299 Practice for Applying Statistical Quality Assurance
sulfur level of various petroleum products and additives. This
and Control Charting Techniques to Evaluate Analytical
knowledge can be used to predict performance, handling, or
Measurement System Performance
processing properties. In some cases the presence of sulfur
compounds is beneficial to the product and monitoring the
depletion of sulfur can provide useful information. In other
1 cases the presence of sulfur compounds is detrimental to the
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
processing or use of the product.
Subcommittee D02.03 on Elemental Analysis.
Current edition approved June 15, 2014. Published July 2014. Originally
5. Interferences
approved in 1958. Last previous edition approved in 2008 as D1552–08. DOI:
10.1520/D1552-08R14.
5.1 For the iodate systems, chlorine in concentrations less
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
than 1 mass % does not interfere. The IR system can tolerate
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
somewhat higher concentrations. Nitrogen when present in
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. excessof0.1mass %mayinterferewiththeiodatesystems;the
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1552 − 08 (2014)
extent of such interference may be dependent on the type of
nitrogen compound as well as the combustion conditions.
Nitrogen does not interfere with the IR system. The alkali and
alkaline earth metals, as well as zinc, phosphorus, and lead, do
not interfere with either system.
6. Apparatus
6.1 Combustion and Iodate Detection System:
6.1.1 Furnaces—Twomajortypesareavailable,theprimary
difference being the manner in which the necessary high
temperatures are obtained. These two types are as follows:
6.1.1.1 Induction Type, which depends upon the high-
frequency electrical induction method of heating. This assem-
bly shall be capable of attaining a temperature of at least
1482°C (2700°F) in the sample combustion zone, under the
conditions set forth in 9.1 and shall be equipped with an
FIG. 1 Combustion Tube
additional induction coil located above the combustion zone,
substantially as shown in Fig. 1.
6.1.1.2 The furnace work coil should have a minimum
outputof500 W;theminimuminputratingofthefurnacemust
6.4 Sieve, 60-mesh (250-mm).
be 1000 W. With the correct amount of iron chips, weighed to
60.05 g, the maximum plate current will be between 350 and
7. Reagents and Materials
450 mA. (Warning—This type of furnace is capable of
7.1 Purity of Reagents—Reagent grade chemicals shall be
inflicting high frequency burns and high-voltage shocks. In
used in all tests. Unless otherwise indicated, it is intended that
addition to other precautions, maintain all guards properly.)
all reagents shall conform to the specifications of the Commit-
(Warning—Disconnect the furnace from the power line when-
tee onAnalytical Reagents of theAmerican Chemical Society,
ever electrical repairs or adjustments are made.)
where such specifications are available. Other grades may be
6.1.1.3 Resistance Type, capable of maintaining a tempera-
used, provided it is first ascertained that the reagent is of
ture of at least 1371°C (2500°F).
sufficiently high purity to permit its use without lessening the
6.1.2 Absorber, as described in Test Method D1266.
accuracy of the determination.
NOTE 1—Also suitable for use with either type of furnace is an
7.2 Purity of Water—Unless otherwise indicated, references
automatic titrator, specifically designed for iodometry. This combines the
functions of absorption and titration to a predetermined end point.
to water shall be understood to mean reagent water as defined
by Type II or III of Specification D1193.
6.1.3 Buret, standard 25-mL or automatic types available
from the manufacturers of the specific combustion units, are
7.3 Alundum (Al O )or Magnesium Oxide (Com-Aid).
2 3
suitable (Note 1).
7.4 Anhydrone (Magnesium Perchlorate). (Warning—In
6.2 Combustion and IR Detection System, comprised of
addition to other precautions, handle magnesium perchlorate
automatic balance, oxygen flow controls, drying tubes, com-
with care.Avoid contacting it with acid and organic materials.
bustion furnace, infrared detector and microprocessor. The
Reactions with fuel may be violent.)
furnace shall be capable of maintaining a nominal operating
7.5 Hydrochloric Acid (3 + 197)—Dilute 30 mL of concen-
temperature of 1350°C (2460°F).
tratedhydrochloricacid(HCl,relativedensity1.19)to2Lwith
6.3 Miscellaneous Apparatus—Specific combustion assem-
water. (Warning—Poison. Corrosive. May be fatal if swal-
blies require additional equipment such as crucibles, combus-
lowed. Liquid and vapor cause severe burns.)
tion boats, crucible lids, boat pushers, separator disks, com-
7.6 Oxygen (Extra Dry)—The oxygen shall be at least
bustion tubes, sample inserters, oxygen flow indicator, and
99.5 % pure and show no detectable sulfur by blank determi-
oxygen drying trains. The additional equipment required is
nation. (Warning—Oxygen vigorously accelerates combus-
dependentonthetypeoffurnaceusedandisavailablefromthe
tion.)
manufacturer of the specific combustion unit. To attain the
7.7 Phosphorus Pentoxide—(P O ).
lower sulfur concentration given in Section 1, the ceramics
2 5
used with the induction furnace assembly shall be ignited in a
7.8 Potassium Alum (Aluminum Potassium Sulfate).
muffle furnace at 1371°C (2500°F) for at least 4 h before use.
Reagent Chemicals, American Chemical Society Specifications, American
The sole source of supply of Models SC32 or SC132 known to the committee Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
at this time is LECO Corp., 3800 LakeviewAve., St. Joseph, MI 49085-2396. If you listed by the American Chemical Society, see Annual Standards for Laboratory
are aware of alternative suppliers, please provide this information to ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
International Headquarters. Your comments will receive careful consideration at a and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
meeting of the responsible technical committee, which you may attend. MD.
D1552 − 08 (2014)
7.9 Potassium Iodate, Standard Solution (0.06238 N), 1 mL
of this solution is equivalent to 1 mg S)—Dissolve 2.225 g of
potassium iodate (KIO ) that has been dried at about 180°C to
constantweight,inwateranddiluteto1L.Thoroughlymixthe
solution.
7.10 Potassium Iodate, Standard Solution (0.006238 N),
1 mL of this solution is equivalent to 0.1 mg S)—Measure
exactly 100 mL of KIO solution (0.06238 N) into a 1–L
FIG. 2 Schematic Illustration of Induction-Type Furnace
volumetric flask, and dilute to volume with water. Thoroughly
mix the solution.
7.11 Potassium Iodate, Standard Solution (0.01248 N),
starch-iodide solution to the absorber.Add a sufficient amount
1 mL of this solution is equivalent to 0.2 mg S)—Measure
of the appropriate standard KIO solution (Table 1) to produce
exactly 200 mL of KIO solution (0.06238 N) into a 1-L
a faint blue color. This color will serve as the end point for the
volumetric flask and dilute to volume with water. Thoroughly
titration.Adjust the buret to zero. Turn on the furnace filament
mix the solution.
switch and allow at least 1 min warm-up before running
7.12 Ascarite, 8 to 20 mesh. samples (Warning—see 7.4).
9.2 Resistance–Type Furnace—Assemble the apparatus ac-
7.13 Special Materials for Induction-Type Furnaces:
7.13.1 Tin (20 to 30-mesh). cording to the instructions furnished by the manufacturer.
Purify the oxygen by passing it through (1)H SO (relative
7.13.2 Iron-Chip Accelerator having a sulfur content of not
2 4
more than 0.005 mass %. density 1.84), (2) Ascarite, and (3) Mg(ClO ) or P O
4 2 2 5
(Warning—see 7.4). Connect a rotameter between the purify-
7.14 Standard Sample—Potassium alum (AlK(SO ) ·
4 2
ing train and the furnace. Fig. 3 illustrates schematically the
12H O).
assembled apparatus. Turn on the current and adjust the
7.15 Starch-Iodide Solution—Make a paste by adding9gof
furnace control to maintain a constant temperature of
soluble starch to 15 mL of water. Add this mixture, with
1316 6 14°C (2400 6 25°F). Adjust the oxygen flow rate to
stirring,to500 mLofboilingwater.Coolthemixture,add15 g
2 6 0.1 L/min. Add 65 mL of HCl (3 6 197) and 2 mL of
of potassium iodide (KI), and dilute to 1 L with water.
starch-iodide solution to the absorber. Add a few drops of the
appropriate standard KIO solution (Table 2) to produce a faint
7.16 Sulfuric Acid (relative density 1.84)—Concentrated
blue color. Adjust the buret to zero.
sulfuric acid (H SO ). (Warning—Poison. Corrosive. Strong
2 4
oxidizer.)
9.3 Resistance–Type Furnace–IR Detection—Assemble and
adjust apparatus according to manufacturer’s instructions.
7.17 Vanadium Pentoxide, anhydrous, powdered V O .
2 5
Initialize microprocessor, check power supplies, set oxygen
7.18 Quality Control (QC) Sample(s) , preferably are por-
pressure and flows and set furnace temperature to 1371°C
tions of one or more petroleum products that are stable and
(2500°F).
representative of the samples of interest. These QC samples
9.3.1 Condition a fresh anhydrone scrubber with four coal
can be used to check the validity of the testing process and
samples when analyzing petroleum coke samples, or with four
performance of the instrument as described in Section 12.
petroleum product samples that are representative or typical of
the sample types to be analyzed.
8. Sampling
9.3.2 Calibrate the automatic balance according to manu-
8.1 Take samples in accordance with the instructions in
facturer’s instructions.
Practice D4057.
10. Standardization
9. Preparation of Apparatus
10.1 For Iodate Methods:
9.1 Induction-Type Furnace—Assemble the apparatus ac- 10.1.1 Determination of Alum Factor:
cording to the instructions furnished by the manufacturer. 10.1.1.1 Because these rapid combustion methods involve
Purify the oxygen by passing it through (1)H SO (relative the reversible reaction 2SO +O = 2SO , it is not possible to
2 4 2 2 3
density 1.84), ( 2) Ascarite, and (3) magnesium perchlorate evolve all the sulfur as SO . The equilibrium of the reaction is
(Mg(ClO ) ) or phosphorus pentoxide (P O)(Warning—see temperature dependent and, in an oxygen atmosphere above
4 2 2 5
7.4). Connect a rotameter between the purifying train and the 1316°C, about 97 % of the sulfur is present as SO . To assure
furnace. Insert a small glass-wool plug in the upper end of the that the furnace is in proper adjustment and that its operation
glass tubing connecting the furnace with the absorber to catch produces acceptably high temperature, potassium alum is
oxides of tin. Connect the exit end of the combustion tube to employed for standardizing the apparatus. Depending on the
the absorber with glass tubing, using gum rubber tubing to type of combustion equipment used, proceed as described in
make connections. Position the absorber so as to make this Sections 10 to 14 to determine the alum factor. Use 15 mg
delivery line as short as possible. Fig. 2 illustrates schemati- weighed to 60.1 mg of potassium alum for
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D1552 − 08 D1552 − 08 (Reapproved 2014)
Standard Test Method for
Sulfur in Petroleum Products (High-Temperature Method)
This standard is issued under the fixed designation D1552; 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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope*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 177°C (350°F) 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 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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:
D1193 Specification for Reagent Water
D1266 Test Method for Sulfur in Petroleum Products (Lamp Method)
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories
3. Summary of Test Method
3.1 Iodate Detection System—The sample is burned in a stream of oxygen at a sufficiently high temperature to convert about
97 % of the sulfur to sulfur dioxide. A standardization factor is employed to obtain accurate results. The combustion products are
passed into an absorber containing an acid solution of potassium iodide and starch indicator. A faint blue color is developed in the
absorber solution by the addition of standard potassium iodate solution. As combustion proceeds, bleaching the blue color, more
iodate is added. The amount of standard iodate consumed during the combustion is a measure of the sulfur content of the sample.
3.2 IR Detection System—The sample is weighed into a special ceramic boat which is then placed into a combustion furnace
at 1371°C (2500°F) in an oxygen atmosphere. Most sulfur present is combusted to SO which is then measured with an infrared
detector after moisture and dust are removed by traps. A microprocessor calculates the mass percent sulfur from the sample weight,
the integrated detector signal and a predetermined calibration factor. Both the sample identification number and mass percent sulfur
are then printed out. The calibration factor is determined using standards approximating the material to be analyzed.
4. Significance and Use
4.1 This test method provides a means of monitoring the sulfur level of various petroleum products and additives. This
knowledge can be used to predict performance, handling, or processing properties. In some cases the presence of sulfur compounds
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
Current edition approved Dec. 1, 2008June 15, 2014. Published December 2008July 2014. Originally approved in 1958. Last previous edition approved in 20072008 as
D1552–07.–08. DOI: 10.1520/D1552-08.10.1520/D1552-08R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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
D1552 − 08 (2014)
is beneficial to the product and monitoring the depletion of sulfur can provide useful information. In other cases the presence of
sulfur compounds is detrimental to the processing or use of the product.
5. Interferences
5.1 For the iodate systems, chlorine in concentrations less than 1 mass % does not interfere. The IR system can tolerate
somewhat higher concentrations. Nitrogen when present in excess of 0.1 mass % may interfere with the iodate systems; the extent
of such interference may be dependent on the type of nitrogen compound as well as the combustion conditions. Nitrogen does not
interfere with the IR system. The alkali and alkaline earth metals, as well as zinc, phosphorus, and lead, do not interfere with either
system.
6. Apparatus
6.1 Combustion and Iodate Detection System:
6.1.1 Furnaces—Two major types are available, the primary difference being the manner in which the necessary high
temperatures are obtained. These two types are as follows:
6.1.1.1 Induction Type, which depends upon the high-frequency electrical induction method of heating. This assembly shall be
capable of attaining a temperature of at least 1482°C (2700°F) in the sample combustion zone, under the conditions set forth in
9.1 and shall be equipped with an additional induction coil located above the combustion zone, substantially as shown in Fig. 1.
6.1.1.2 The furnace work coil should have a minimum output of 500 W; the minimum input rating of the furnace must be 1000
W. With the correct amount of iron chips, weighed to 60.05 g, the maximum plate current will be between 350 and 450 mA.
(Warning—This type of furnace is capable of inflicting high frequency burns and high-voltage shocks. In addition to other
precautions, maintain all guards properly.) (Warning—Disconnect the furnace from the power line whenever electrical repairs or
adjustments are made.)
6.1.1.3 Resistance Type, capable of maintaining a temperature of at least 1371°C (2500°F).
6.1.2 Absorber, as described in Test Method D1266.
NOTE 1—Also suitable for use with either type of furnace is an automatic titrator, specifically designed for iodometry. This combines the functions of
absorption and titration to a predetermined end point.
6.1.3 Buret, standard 25-mL or automatic types available from the manufacturers of the specific combustion units, are suitable
(Note 1).
6.2 Combustion and IR Detection System, comprised of automatic balance, oxygen flow controls, drying tubes, combustion
furnace, infrared detector and microprocessor. The furnace shall be capable of maintaining a nominal operating temperature of
1350°C (2460°F).
FIG. 1 Combustion Tube
6.3 Miscellaneous Apparatus—Specific combustion assemblies require additional equipment such as crucibles, combustion
boats, crucible lids, boat pushers, separator disks, combustion tubes, sample inserters, oxygen flow indicator, and oxygen drying
trains. The additional equipment required is dependent on the type of furnace used and is available from the manufacturer of the
The sole source of supply of Models SC32 or SC132 known to the committee at this time is LECO Corp., 3800 Lakeview Ave., St. Joseph, MI 49085-2396. If you are
aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend.
D1552 − 08 (2014)
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 1371°C (2500°F) for at least 4 h before use.
6.4 Sieve, 60-mesh (250-mm).
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
7.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by
Type II or III of Specification D1193.
7.3 Alundum (Al O ) or Magnesium Oxide (Com-Aid).
2 3
7.4 Anhydrone (Magnesium Perchlorate) . Perchlorate). (Warning—In addition to other precautions, handle magnesium
perchlorate with care. Avoid contacting it with acid and organic materials. Reactions with fuel may be violent.)
7.5 Hydrochloric Acid (3 + 197)—Dilute 30 mL of concentrated hydrochloric acid (HCl, relative density 1.19) to 2 L with water.
(Warning—Poison. Corrosive. May be fatal if swallowed. Liquid and vapor cause severe burns.)
7.6 Oxygen (Extra Dry)—The oxygen shall be at least 99.5 % pure and show no detectable sulfur by blank determination.
(Warning—Oxygen vigorously accelerates combustion.)
7.7 Phosphorus Pentoxide—(P O ).
2 5
7.8 Potassium Alum (Aluminum Potassium Sulfate).
7.9 Potassium Iodate, Standard Solution (0.06238 N), 1 mL of this solution is equivalent to 1 mg S)—Dissolve 2.225 g of
potassium iodate (KIO ) that has been dried at about 180°C to constant weight, in water and dilute to 1 L. Thoroughly mix the
solution.
7.10 Potassium Iodate, Standard Solution (0.006238 N), 1 mL 1 mL of this solution is equivalent to 0.1 mg 0.1 mg S)—Measure
exactly 100 mL of KIO solution (0.06238 N) into a 1–L volumetric flask, and dilute to volume with water. Thoroughly mix the
solution.
7.11 Potassium Iodate, Standard Solution (0.01248 N), 1 mL 1 mL of this solution is equivalent to 0.2 mg 0.2 mg S)—Measure
exactly 200 mL of KIO solution (0.06238 N) into a 1-L volumetric flask and dilute to volume with water. Thoroughly mix the
solution.
7.12 Ascarite, 8 to 20 mesh.
7.13 Special Materials for Induction-Type Furnaces:
7.13.1 Tin (20 to 30-mesh).
7.13.2 Iron-Chip Accelerator having a sulfur content of not more than 0.005 mass %.
7.14 Standard Sample—Potassium alum (AlK(SO ) · 12H O).
4 2 2
7.15 Starch-Iodide Solution—Make a paste by adding 9 g of soluble starch to 15 mL 15 mL of water. Add this mixture, with
stirring, to 500 mL 500 mL of boiling water. Cool the mixture, add 15 g 15 g of potassium iodide (KI), and dilute to 1 L 1 L with
water.
7.16 Sulfuric Acid (relative density 1.84)—Concentrated sulfuric acid (H SO ). (Warning—Poison. Corrosive. Strong
2 4
oxidizer.)
7.17 Vanadium Pentoxide, anhydrous, powdered V O .
2 5
7.18 Quality Control (QC) Sample(s) , preferably are portions of one or more petroleum products that are stable and
representative of the samples of interest. These QC samples can be used to check the validity of the testing process and
performance of the instrument as described in Section 12.
8. Sampling
8.1 Take samples in accordance with the instructions in Practice D4057.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed by
the American Chemical Society, see Annual 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.
D1552 − 08 (2014)
FIG. 2 Schematic Illustration of Induction-Type Furnace
9. Preparation of Apparatus
9.1 Induction-Type Furnace—Assemble the apparatus according to the instructions furnished by the manufacturer. Purify the
oxygen by passing it through (1) H SO (relative density 1.84), ( 2) Ascarite, and (3) magnesium perchlorate (Mg(ClO ) ) or
2 4 4 2
phosphorus pentoxide (P O ) (Warning—see 7.4). Connect a rotameter between the purifying train and the furnace. Insert a small
2 5
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 KIO 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 (Warning—see 7.4).
9.2 Resistance–Type Furnace—Assemble the apparatus according to the instructions furnished by the manufacturer. Purify the
oxygen by passing it through (1) H SO (relative density 1.84), (2) Ascarite, and (3) Mg(ClO ) or P O (Warning—see 7.4).
2 4 4 2 2 5
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 14°C (2400 6 25°F).
1316 6 14°C (2400 6 25°F). Adjust the oxygen flow rate to 2 6 0.1 2 6 0.1 L/min. Add 65 mL 65 mL of HCl (3 6 197) and 2
mL (3 6 197) and 2 mL of starch-iodide solution to the absorber. Add a few drops of the appropriate standard KIO solution (Table
2) to produce a faint blue color. Adjust the buret to zero.
9.3 Resistance–Type Furnace–IR Detection —Detection—Assemble and adjust apparatus according to manufacturer’s instruc-
tions. Initialize microprocessor, check power supplies, set oxygen pressure and flows and set furnace temperature to 1371°C
(2500°F).
9.3.1 Condition a fresh anhydrone scrubber with four coal samples when analyzing petroleum coke samples, or with four
petroleum product samples that are representative or typical of the sample types to be analyzed.
9.3.2 Calibrat
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.