Designation: D 3227 – 99 An American National Standard

Designation: 342/93
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM

Standard Test Method for

Thiol (Mercaptan) Sulfur in Gasoline, Kerosine, Aviation
Turbine, and Distillate Fuels (Potentiometric Method)1
This standard is issued under the fixed designation D 3227; 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.

This standard has been approved for use by agencies of the Department of Defense.
This test method has been approved by the sponsoring committee and accepted by the cooperation societies in accordance with
established procedures.

1. Scope Petroleum Products4

1.1 This test method covers the determination of mercaptan D 6299 Practice for Applying Statistical Quality Assurance
sulfur in gasolines, kerosines, aviation turbine fuels, and Techniques to Evaluate Analytical Measurement System
distillate fuels containing from 0.0003 to 0.01 mass % of Performance5
mercaptan sulfur. Organic sulfur compounds such as sulfides, 3. Summary of Test Method
disulfides, and thiophene, do not interfere. Elemental sulfur in
amounts less than 0.0005 mass % does not interfere. Hydrogen 3.1 The hydrogen sulfide-free sample is dissolved in an
sulfide will interfere if not removed, as described in 9.2. alcoholic sodium acetate titration solvent and titrated potentio-
1.2 The values in acceptable SI units are to be regarded as metrically with silver nitrate solution (see Note 4), using as an
the standard. The values in parentheses are for information indicator the potential between a glass reference electrode and
only. a silver/silver-sulfide indicating electrode. Under these condi-
1.3 This standard does not purport to address all of the tions, the mercaptan sulfur is precipitated as silver mercaptide
safety concerns, if any, associated with its use. It is the and the end point of the titration is shown by a large change in
responsibility of the user of this standard to establish appro- cell potential.
priate safety and health practices and determine the applica- 4. Significance and Use
bility of regulatory limitations prior to use. For specific hazard
statements, see Note 1, Note 2, Note 3, Note 5, and Note 6. 4.1 Mercaptan sulfur has an objectionable odor, an adverse
effect on fuel system elastomers, and is corrosive to fuel
2. Referenced Documents system components.
2.1 ASTM Standards: 5. Apparatus
D 1193 Specification for Reagent Water2
D 1250 Guide for Petroleum Measurement Tables3 5.1 As described in 5.2-5.5; alternatively, any automatic
D 1298 Test Method for Density, Relative Density (Specific titration system may be used that, using the same electrode pair
Gravity), or API Gravity of Crude Petroleum and Liquid described in 5.3, is capable of performing the titration as
Petroleum Products by Hydrometer Method3 described in Section 9 and selecting the endpoint specified in
D 4052 Test Method for Density and Relative Density of 11.1 with a precision that meets or is better than that given in
Liquids by Digital Density Meter4 Section 13.
D 4057 Practice for Manual Sampling of Petroleum and 5.2 Meter—An electronic voltmeter, operating on an input
Petroleum Products4 of less than 9 3 10−12 A and having a sensitivity of 62 mV
D 4177 Practice for Automatic Sampling of Petroleum and over a range of at least 61 V. The meter shall be electrostati-
cally shielded, and the shield shall be connected to the ground.6
5.3 Cell System, consisting of a reference and indicating
1
This test method is under the jurisdiction of ASTM Committee D-2 on electrode. The reference electrode should be a sturdy, pencil-
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee type glass electrode, having a shielded lead connected to
D02.03 on Elemental Analysis. ground. The indicating electrode shall be made from a silver
Current edition approved Jan. 10, 1999. Published March 1999. Originally
published as D 3227 – 73. Last previous edition D 3227 – 96e1.
2
Annual Book of ASTM Standards, Vol 11.01.
3 5
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 05.03.
4 6
Annual Book of ASTM Standards, Vol 05.02. Any apparatus that will give equal or better precision will be acceptable.

1
D 3227
wire, 2 mm (0.08 in.) in diameter or larger, mounted in an NOTE 4—It is important to pass the propan-2-ol through a column of
insulated support. Silver billet electrodes can also be used. activated alumina to remove peroxides that may have formed on storage;
5.4 Buret, 10-mL capacity, graduated in 0.05-mL intervals, failure to remove peroxides will lead to low results. It is not necessary to
perform this step if the alcohol is tested and found free of peroxides.
with a tip that extends approximately 120 mm (5 in.) below the
stopcock. 6.6.1 Standardization—Add six drops of concentrated
5.5 Titration Stand, preferably built as an integral part of the HNO3(rel dens 1.42) (Warning—See Note 5) to 100 mL of
meter housing and provided with supports for the electrodes water in a 300-mL tall-form beaker. Remove oxides of nitrogen
and electrical stirrer, all connected to ground. No permanent by boiling for 5 min. Cool to ambient temperature. Pipet 5 mL
change in meter reading should be noticeable upon connecting of 0.1 mol/L KI solution into the beaker and titrate with the
or disconnecting the stirring motor. AgNO3 solution choosing the end point at the inflection of the
6. Reagents and Materials titration curve.
6.1 Purity of Reagents—Reagent grade chemicals shall be NOTE 5—Warning: Poison. Causes severe burns. Harmful or fatal if
used in all tests. Unless otherwise indicated, it is intended that swallowed or inhaled.
all reagents shall conform to the specifications of the Commit-
6.7 Silver Nitrate, Standard Alcoholic Solution (0.010 mol/
tee on Analytical Reagents of the American Chemical Society,
L)—Prepare daily when the test is being performed by dilution
where such specifications are available.7 Other grades may be
of the 0.1 N standard. Pipet 100 mL of the 0.1 mol/L standard
used, provided it is first ascertained that the reagent is of
into a 1-L volumetric flask and dilute to volume with propan-
sufficiently high purity to permit its use without lessening the
2-ol. Calculate the exact molarity.
accuracy of the determination.
6.1.1 Commercially available solutions may be used in 6.8 Sodium Sulfide Solution (10 g/L)—Dissolve 10 g of
place of prepared laboratory solutions, when they are certified Na2S in water and dilute to 1 L with water. Prepare fresh as
to meet the required concentrations. needed.
6.1.2 Alternate volumes of solutions and solvents may be 6.9 Sulfuric Acid, dilute. Cautiously dilute five volumes of
prepared, when an equivalent concentration is maintained. water with one volume of sulfuric acid (Sp.Gr.1.84). (Precau-
6.2 Water—Reagent grade, Type I, Specification D 1193. tions: Adding the acid will generate heat: mix well. If water
6.3 Cadmium Sulfate, Acid Solution (150 g/L)—Dissolve begins to boil, cool before adding more acid. Note that only
150 g of cadmium sulfate (3CdSO4 3 8H2O) in water. limited volumes are required because only 10 mL are needed
(Warning—See Note 1) Add 10 mL of dilute for each litre of cadmium sulfate solution.
H2SO4(Warning—See Note 2) and dilute to 1 L with water. 6.10 Titration Solvent—Low molecular weight mercaptans,
NOTE 1—Warning: Poison. May be fatal if swallowed or inhaled. A as usually found in gasoline, are readily lost from the titration
known carcinogen (animal positive). solution if an acidic titration solvent is used. For the determi-
NOTE 2—Warning—Poison. Causes severe burns. Harmful or fatal if nation of the higher molecular weight mercaptan as normally
swallowed or inhaled. encountered in kerosines, aviation turbine fuels, and distillate
6.4 Potassium Iodide, Standard Solution (approximately 0.1 fuels, the acidic titration solvent is used to achieve more rapid
mol/L)—Dissolve 17 g of KI (weigh to 0.01 g) in 100 mL of equilibrium between successive additions of the titrant.
water in a 1-L volumetric flask and dilute to 1 L. Calculate the 6.10.1 Alkaline Titration Solvent—Dissolve 2.7 g of sodium
exact molarity. acetate trihydrate (NaC2H3O2·3H2O) or 1.6 g of anhydrous
6.5 2-Propanol—(Warning—See Note 3). Precaution— sodium acetate (NaC2H3O2) in 25 mL of water free of
Unless inhibited against it, peroxides can form in 2-propanol dissolved oxygen and pour into 975 mL of propan-2-ol (99 %)
when stored in the same container that is exposed to air. When (Note 4). When necessary, remove dissolved oxygen by purg-
this happens and the propan-2-ol evaporates to dryness, an ing the solution with a rapid stream of nitrogen for 10 min each
explosion can occur. When peroxides are suspected, they may day prior to use; keep protected from the atmosphere. To
be removed by percolation through an activated alumina minimize oxygen from dissolving in the solution during
column. storage, an option exists to nitrogen blanket the solution prior
NOTE 3—Warning: Flammable. to sealing the solvent container.
6.6 Silver Nitrate, Standard Alcoholic Solution (0.1 mol/ 6.10.2 Acidic Titration Solvent—Dissolve 2.7 g of
L)—Dissolve 17 g of AgNO3 in 100 mL of water in a 1-L NaC2H3O2·3H2O or 1.6 g of NaC2H3O2 in 20 mL of water free
volumetric flask and dilute to 1 L with 2-propanol (99 %) (see of dissolved oxygen and pour into 975 mL of propan-2-ol
Note 4). Store in a dark bottle and standardize at intervals (99 %) (Note 4) and add 4.6 mL of glacial acetic acid. When
frequent enough to detect a change of 0.0005 or greater in necessary, remove dissolved oxygen by purging the solution
molarity. with a rapid stream of nitrogen for 10 min each day prior to
use; keep protected from the atmosphere. To minimize oxygen
7
Reagent Chemicals, American Chemical Society Specifications, American from dissolving in the solution during storage, an option exists
Chemical Society, Washington, DC. For suggestions on the testing of reagents not to nitrogen blanket the solution prior to sealing the solvent
listed by the American Chemical Society, see Analar Standards for Laboratory container.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, 6.11 Polishing Paper or Cloth, 16–20 µm average particle
MD. size abrasive.

2
D 3227
7. Sampling the water after each washing. Filter the hydrocarbon through a
7.1 Take the sample in accordance with Practice D 4057 or rapid paper. Test a small portion of the washed sample in a test
Practice D 4177. tube with a few millilitres of the CdSO4 solution. If no further
7.2 Methanethiol (methyl mercaptan) has a boiling point of precipitate is formed, proceed as directed in 9.3. If a precipitate
6.2°C and may be expected to be present in light untreated appears, repeat the extraction with the CdSO4 solution until all
gasolines. Therefore, when the presence of this low boiling of the H2S has been removed.
thiol (mercaptan) is known or expected, specimen to be tested NOTE 7—Caution: Certain straight run gasolines can contain signifi-
shall be kept below 4°C to prevent the loss of mercaptan from cant amounts of both low molecular weight mercaptans and dissolved
such samples. elemental sulfur, which, when heated under total reflux conditions, may
produce H2S by the inter-reaction of both. This phenomenon is particu-
8. Preparation of Apparatus larly noticed in straight run gasolines produced from some natural gas
condensates. Therefore, it is advisable that during the removal of H2S (and
8.1 Glass Electrode—After each manual titration, or batch after all H2S has been extracted), that no heat should be applied to the
of titrations, in the case of automatic titration systems, wipe the sample.
electrode with a soft, clean tissue and rinse with water. Clean 9.2.1 When the test results obtained are not for referee
the electrode at frequent intervals (at least once a week) by purposes and Quality Assurance/Quality Control (QA/QC)
stirring in cold chromic acid solution (Warning—See Note 6) protocol permits, an alternative test for, and a procedure for the
for a few seconds (10 s maximum). When not in use, keep removal of, hydrogen sulfide can be used. This process uses
lower half of the electrode immersed in water. lead acetate paper and sodium hydrogen carbonate and is
NOTE 6—Warning: Causes severe burns. A recognized carcinogen. described in Appendix X1.
Strong oxidizer—contact with other material may cause fire. Hygroscopic. 9.2.2 For referee purposes, the protocol, as detailed in 9.2,
An equivalent, chromium-free cleaning solution may be used. shall be used. A possible non-referee situation may be the
8.2 Silver/Silver-Sulfide Electrode—Each day prior to use, instance of routine refinery control.
prepare a fresh silver sulfide coating on the electrode by the 9.3 Measure with a pipet or weigh 20 to 50 mL of the
following method: original or treated sample into a 300-mL beaker containing 100
8.2.1 Burnish electrode with polishing paper or cloth until a mL of the appropriate titration solvent. Place the beaker on the
clean, polished silver surface shows. titration stand or on the auto-sampler of an automatic titration
8.2.2 Place electrode in operating position and immerse it in system. If an automatic titration system is used, set up the
100 mL of titration solvent containing 8 mL of Na2S solution. system to reproduce the experimental conditions specified in
8.2.3 Add slowly from a buret, with stirring, 10 mL of 0.1 9.3.1, 9.3.2, and 9.3.3. Adjust the position of the titration stand
mol/L AgNO3 solution over a period from 10 to 15 min. so that the electrodes are about half immersed. Fill the buret
8.2.4 Remove electrode from solution, wash with water, and with 0.01 mol/L alcoholic AgNO3 solution and position it in
wipe with a soft, clean tissue. the titration assembly so that the tip extends approximately 25
8.2.5 Between manual titrations, or batches of titrations in mm (1 in.) below the surface of the liquid in the beaker. Adjust
the case of automatic titration systems, store the electrode a the speed of the stirrer to give vigorous stirring without
minimum of 5 min in 100 mL of titration solvent containing 0.5 spattering.
mL of the 0.1 mol/L AgNO3 solution. 9.3.1 Record the initial buret and cell potential readings.
The usual meter readings for mercaptan presence are in
9. Procedure the −250 mV to −350 mV range. Add suitable small portions of
9.1 Determination of Density—If the sample is to be mea- 0.01 mol/L AgNO3 solution and, after waiting until a constant
sured volumetrically, determine the density by Test Method potential has been established, record the buret and meter
D 1298 or D 4052 at the temperature at which the test portion readings. Consider the potential constant if it changes less than
will be taken, either directly or from the density determined at 6 mV/min.
a reference temperature and converted to the transfer tempera- NOTE 8—If potential readings obtained with freshly prepared electrodes
ture by use of the Petroleum Measurement Tables (Guide are erratic, it is possible that the electrodes are not properly conditioned.
D 1250). This difficulty usually disappears in succeeding titrations.
9.2 Removal of Hydrogen Sulfide—Test the sample qualita- NOTE 9—With certain instruments, the algebraic sign of the potentials
tively for hydrogen sulfide (H2S) by shaking 5 mL of the may appear reversed.
sample with 5 mL of the acid CdSO4 solution. If no precipitate 9.3.2 When the potential change is small for each increment
appears, proceed with the analysis of the sample as described of AgNO3 solution, add volumes as large as 0.5 mL. When the
in 9.3. If a yellow precipitate appears, remove the H2S in the change of potential becomes greater than 6 mV/0.1 mL, use
following manner: Place a quantity of the sample, three to four 0.05-mL increments of 0.01 mol/L AgNO3 solution. Near the
times that required for the analysis, in a separatory funnel end point of the titration, 5 or 10 min may elapse before a
containing a volume of the acid CdSO4 solution equal to one constant potential is obtained. Although it is important to wait
half that of the sample and shake vigorously. Draw off and for equilibrium conditions, it is also important that the duration
discard the aqueous phase containing the yellow precipitate. of the titration be as short as possible to avoid oxidation of the
Repeat the extraction with another portion of the CdSO4 sulfur compounds by atmospheric oxygen. Once started, a
solution. Again draw off the aqueous phase, and wash the titration must never be interrupted and resumed later.
sample with three 25 to 30-mL portions of water, withdrawing 9.3.3 Continue the titration until the meter reading change

3
D 3227
of the cell potential per 0.1 mL of 0.01 M AgNO3 solution has
become relatively constant. Consider the potential constant if it
changes less than 6 mV/min. Remove the titrated solution,
rinse the electrodes with alcohol, and wipe with a dry tissue. If
an automatic titration system is used, rinse the electrodes well
with alcohol, allow the excess alcohol to drain off the electrode
and then proceed with the next sample. Between successive
determinations (or batches of determinations in the case of
automatic titration systems) on the same day, store the elec-
trodes in accordance with 8.1 and 8.2.5.
9.4 As often as is required and preferably, at least daily,
when the test equipment is being used, perform a blank
titration following 9.3-9.3.3 without adding a test sample.
10. Calculation
10.1 Calculate the mercaptan sulfur content of the sample as
follows:
Mercaptan sulfur, mass % 5 ~AM ~A1 – A0!3 3.206!/W (1)
or FIG. 1 Illustrative Potentiometric Titration Curves
Mercaptan sulfur, mass % 5 ~AM ~A1 – A0! 3 3.206!/~d 3 V!
(2)
equivalent amount of mercaptan, the total titration to the
where: mercaptide end point must be used to calculate the amount of
A1 5 millilitres of AgNO3 solution required to reach the mercaptan sulfur.
end point in the vicinity of +300 mV (see Fig. 1), 11.1.4 When elemental sulfur is present in excess, the end of
when a sample is being titrated, the Ag2S precipitation is taken in the same region ( +300 mV)
A0 5 mL of AgNO3 solution required to reach the end as in the case of silver mercaptide, and is calculated as
point in the vicinity of +300mV (see Fig. 1), when mercaptan sulfur.
only the blank is titrated. (Note, there are no other 11.1.5 When samples of light gasolines containing meth-
changes to the factors in the equation). anethiol (methyl mercaptan) or heavier thiols (mercaptans)
d 5 density of sample at transfer temperature, g/mL, appear to give erratic results, it may be necessary to cool and
M 5 molarity of the AgNO3 solution,
maintain the test apparatus below 4°C prior to proceeding, as
W 5 grams of sample used,
3.206 5 100 3 g meq weight S in mercaptan, and detailed in 9.2-9.4 inclusive. For these samples, this step may
V 5 mL of sample used. be necessary for more reproducible test results.

11. Interpretation of Results 12. Quality Assurance/Quality Control

11.1 Treatment of Data—Plot the cumulative volumes of 12.1 Confirm the performance of the instrument and the test
0.01 M AgNO3 solution added against the corresponding cell procedure by analyzing a control (QC) sample.
potentials. Select the end point at the most positive value of the 12.1.1 When QA/QC protocols are already established in
steepest portion of each “break” in the titration curve as shown the testing facility, these may be used when they confirm the
in Fig. 1. The shape of the titration curve may change with reliability of test result.
different instruments. However, the above interpretation of the 12.1.2 When there is no QA/QC protocol established in the
end point should be followed. testing facility, Appendix X2 may be used as the QA/QC
11.1.1 Mercaptans Only—If mercaptans alone are present in system.
the sample, the titration produces a curve of the first type 12.2 Users of this test method are advised that in contractual
shown in Fig. 1, having an initial plateau at a potential equal to agreements, one or more of the contracting parties can and may
or more negative than −250 mV, and an end point when a make Appendix X2 a mandatory practice.
potential change of less than 6 mV/min is reached and the
change in mV/min of titrant is reduced with each incremental 13. Precision and Bias
addition. 13.1 Precision:
11.1.2 Mercaptans and Elemental Sulfur—When elemental 13.1.1 The precision of this test method as determined by
sulfur and mercaptans are both present in the sample, a statistical examination of interlaboratory results is as follows:
chemical interaction occurs which, in the titration solvent used, 13.1.1.1 Repeatability—The difference between two suc-
precipitates silver sulfide (Ag2S) during the titration. cessive test results, obtained by the same operator with the
11.1.3 When mercaptans are present in excess, the end of same apparatus under constant operating conditions on identi-
the Ag2S precipitation occurs at about −550 to −350 mV, and is cal test material, would in the long run, in the normal and
followed by the precipitation of the silver mercaptide to correct operation of the test method, exceed the following
the +300-mV end point. This situation is shown in the middle values only in one case in twenty:
curve of Fig. 1. Since all of the Ag2S originates from an Repeatability 0.00007 + 0.027x (see Note 10)

4
D 3227

where: in twenty:
x 5 average mercaptan sulfur, mass %. Reproducibility 0.00031 + 0.042x (Note 10)
NOTE 10—This amount is shown graphically in Fig. 2. where:
13.1.1.2 Reproducibility—The difference between two x 5 average mercaptan sulfur, mass %.
single and independent results obtained by different operators 13.2 Bias—The bias for the procedure in this test method
working in different laboratories on identical test material has not been determined.
would, in the long run, in the normal and correct operation of 14. Keywords
the test method, exceed the following values only in one case 14.1 mercaptan; potentiometric; sulfur

FIG. 2 Precision Curve for Mercaptan Sulfur in Gasolines, Kerosines, Aviation Turbine, and Distillate Fuels

APPENDIXES

(Nonmandatory Information)

X1. AN ALTERNATIVE METHOD FOR THE REMOVAL OF HYDROGEN SULFIDE

X1.1 Scope X1.2 Summary of Test Method

X1.1.1 This test method provides an alternative to using a X1.2.1 Hydrogen sulfide is detected by saturating strips of
cadmium sulfate acid solution, (see Notes 1 and 2 in main filter paper with lead acetate and drying them prior to use.
procedure). When properly prepared and used, they will turn from a white
X1.1.2 This test method uses lead acetate test paper (Warn- color to a darker color due to the precipitation of lead sulfide
ing: See Note X1.1) to test for the presence of hydrogen sulfide by hydrogen sulfide.
and sodium hydrogen carbonate for the removal of hydrogen X1.2.2 The hydrogen sulfide is removed by repeated wash-
sulfide. ings with an aqueous solution of sodium hydrogen carbonate
until the sample indicates the absence of hydrogen sulfide in
X1.1.3 This test method shall not be used when the sample accordance with the lead acetate test.
is a referee sample or when QA/QC protocols specify the test
method as written. Instances in which they can be used may be X1.3 Reagents and Materials
instances of routine refinery control samples.
X1.3.1 Purity of Reagents—All reagents shall conform to
NOTE X1.1—Warning: Poison, health hazard, may be toxic by inges- the details specified in 6.1 of the main procedure.
tion, inhalation, or absorption through the skin. X1.3.2 Commercially prepared solutions and test paper may

5
D 3227
be used when it is certain they will conform to the specifica- X1.4.2 When the presence of hydrogen sulfide is indicated,
tions detailed in 6.1 of the main procedure. proceed as follows:
X1.3.3 Lead Acetate, Aqueous Solution—Prepare a 5 % X1.4.2.1 Take a portion of the sample that is 3 to 4 times the
(m/m) solution of lead acetate [(CH3COO)2Pb.3H2O] in water. volume required for the actual test and pour it into a separatory
X1.3.4 Lead Acetate, Test Paper—Soak to saturation test funnel.
strips of filter paper in the lead acetate solution and allow to X1.4.2.2 Add a volume of sodium hydrogen carbonate
dry. (Precaution: Since these papers react with hydrogen equal to about half the volume of the test portion and shake
sulfide, it is necessary to dry and store them in a hydrogen thoroughly. (Precaution: When the sample is volatile, release
sulfide free atmosphere.) any pressure developed by the shaking, cautiously.)
X1.3.5 Sodium Hydrogen Carbonate, Aqueous Solution—
X1.4.2.3 Allow the two phases to settle, and when settled,
Prepare this solution by dissolving 50 g 6 1 g of sodium
draw off and discard the aqueous phase.
hydrogen carbonate (Na2HCO3) in water; dilute to 1 L in a
volumetric flask. X1.4.2.4 Test the hydrocarbon phase again with fresh lead
X1.3.6 Test Paper—Any standard laboratory filter paper, acetate paper.
capable of absorbing the lead acetate solution may be used. X1.4.2.5 Continue with the washing process until the
(Precaution: Any paper containing active sulfides will inter- washed sample tests negative to the presence of hydrogen
fere with the test.) sulfide. (Precaution: When elemental sulfur and mercaptans
are both present, it is possible that upon reheating the washed
X1.4 Procedure, Testing and Removal of Hydrogen sample, more hydrogen sulfide will form. Because the forma-
Sulfide tion of more hydrogen sulfide (after washing) will affect the
X1.4.1 Test a small portion of the sample by inserting a test result, do not reheat the washed portion of the sample.)
small strip of lead acetate test paper into it. When the test paper X1.4.2.6 When the test portion is free of all hydrogen
is discolored by turning to a brown or black, the presence of sulfide, the determination of the thiol (mercaptan) content may
hydrogen sulfide is indicated. proceed.

X2. GENERIC QUALITY CONTROL STATEMENT FOR D2 TEST METHODS

X2.1 Confirm the performance of the instrument and the criticality of the quality being measured, the demonstrated
test procedure by analyzing a QC sample. stability of the testing process, and customer requirements.
Generally, a QC sample should be analyzed on each day of
X2.2 Prior to monitoring the measurement process, the user testing routine samples. The QC frequency should be increased
of the method needs to determine the average value and control when a large number of samples are routinely analyzed.
limits of the QC sample.8,9 However, when it is demonstrated that the testing is under
X2.3 Record the QC results and analyze by control charts statistical control, the QC testing frequency may be reduced.
or other statistically equivalent techniques to ascertain the The QC sample precision should be periodically checked
statistical control status of the total testing process.7,8 Any against the ASTM method precision to ensure data quality.
out-of-control data should trigger investigation for root
cause(s). The results of this investigation may, but not neces- X2.5 It is recommended that, when possible, the type of QC
sarily, result in instrument recalibration. sample that is regularly tested be representative of the samples
routinely analyzed. An ample supply of QC sample material
X2.4 In the absence of explicit requirements given in the should be available for the intended period of use and must be
test method, the frequency of QC testing is dependent on the homogeneous and stable under the anticipated storage condi-
tions.
8
Practice D 6299.
9
ASTM MNL7: Manual of Presentation of Data Control Chart Analysis, 6th ed., X2.6 See Footnotes 8 and 9 for further guidance on QC and
Section 3: Control Chart for Individuals, available from ASTM Headquarters. Control Charting techniques.

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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.

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 Headquarters. Your comments will receive careful consideration at a meeting of the responsible
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