An American National Standard

Designation: D 5184 – 01 (Reapproved 2006)

Standard Test Methods for

Determination of Aluminum and Silicon in Fuel Oils by
Ashing, Fusion, Inductively Coupled Plasma Atomic
Emission Spectrometry, and Atomic Absorption
Spectrometry1
This standard is issued under the fixed designation D 5184; 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 Techniques to Evaluate Analytical Measurement System

1.1 These test methods cover the determination of alumi- Performance
num and silicon in fuel oils at concentrations between 5 and E 135 Terminology Relating to Analytical Chemistry for
150 mg/kg for aluminum and 10 and 250 mg/kg for silicon. Metals, Ores, and Related Materials
1.2 Test Method A—Inductively coupled plasma atomic 3. Terminology
emission spectrometry is used in this test method to quantita-
tively determine aluminum and silicon. 3.1 Definition:
1.3 Test Method B—Flame atomic absorption spectrometry 3.1.1 emission spectroscopy—Refer to Terminology E 135.
is used in this test method to quantitatively determine alumi- 3.2 Definitions of Terms Specific to This Standard:
num and silicon. 3.2.1 calibration—the process by which the relationship
1.4 The values stated in SI units are to be regarded as between signal intensity and elemental concentration is deter-
standard. No other units of measurement are included in this mined for a specific element analysis.
standard. 3.2.2 check standard—in calibration, an artifact measured
1.5 This standard does not purport to address all of the periodically, the results of which typically are plotted on a
safety concerns, if any, associated with its use. It is the control chart to evaluate the measurement process.
responsibility of the user of this standard to establish appro- 4. Summary of Test Methods
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific warning 4.1 A weighed quantity of homogenized sample is heated in
statements are given in Sections 7.6, 10.1, and 11.5. a clean platinum dish, the combustible material is removed by
burning and the carbon finally removed by heating in a muffle
2. Referenced Documents furnace at a temperature of 550 6 25°C. The residue is fused
2.1 ASTM Standards: 2 with a lithium tetraborate/lithium fluoride flux. The fused
D 1193 Specification for Reagent Water mixture is digested in a solution of tartaric acid and hydrochlo-
D 4057 Practice for Manual Sampling of Petroleum and ric acid and diluted to volume with water. The resulting
Petroleum Products solution is aspirated into an inductively-coupled plasma and
D 4177 Practice for Automatic Sampling of Petroleum and the emission intensities of aluminum and silicon lines are
Petroleum Products measured. Standard calibration solutions are also aspirated and
D 6299 Practice for Applying Statistical Quality Assurance aluminum and silicon intensities are measured for comparison.
Alternatively, the resulting solution is aspirated into the flame
of an atomic absorption spectrometer and the absorptions of the
1
resonance radiation of aluminum and silicon are measured.
These test methods are under the jurisdiction of ASTM Committee D02 on Standard calibration solutions are also aspirated and aluminum
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
tee D02.03 on Elemental Analysis. and silicon absorption intensities are measured for comparison.
Current edition approved May 1, 2006. Published June 2006. Originally
approved in 1991. Last previous edition approved in 2001 as D 5184 – 01. 5. Significance and Use
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
5.1 Catalyst fines in fuel oils can cause abnormal engine
Standards volume information, refer to the standard’s Document Summary page on wear. These test methods provide a means of determining
the ASTM website. silicon and aluminum, the major constituents of the catalysts.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 D 5184 – 01 (2006)
6. Apparatus NOTE 2—Lithium fluoride is necessary to prevent heavy metal corro-
sion of the platinum dish and to lower the fusion temperature.
6.1 Balance, capable of weighing to 0.1 g, capacity of
150 g. 7.4 Hydrochloric acid (36 % (m/m))—concentrated hydro-
6.2 Choice of Instrument: chloric acid.
6.2.1 Inductively-Coupled Plasma Atomic Emission 7.5 Potassium Hydrogen Sulfate, fused solid.
Spectrometer—Either a sequential or simultaneous spectrom- 7.6 2-Propanol (Isopropyl Alcohol) (Warning—
eter is suitable, if equipped with an ICP torch and RF generator Flammable; can be explosive when evaporated to or near
to form and sustain the plasma. dryness.)
6.2.2 Atomic Absorption Spectrometer—A suitable instru- 7.7 Aqueous Standard Solutions.
ment will consist of modulated hollow cathode lamps or other 7.7.1 Aluminum Standard Solutions—Obtain a ready made,
sources of resonance radiation of aluminum and silicon, a aqueous standard or prepare a standard from aluminum wire.
nitrous oxide/acetylene burner, and a spectrometer with a 7.7.1.1 Aluminum Solution (1000 mg/L)—Aqueous, ready
suitable detection and read-out system. made commercial standard.
6.3 Homogenizer, non-aerating, high-speed shear mixer to 7.7.1.2 Aluminum Solution (1000 mg/L)—Cut an arbitrary
homogenize the sample. length of 99.99 % minimum purity aluminum wire (2 mm
diameter aluminum wire has been found satisfactory). Measure
NOTE 1—Ultrasonic bath and ultrasonic probe type homogenizers were
the length to the nearest 0.1 cm and weigh the aluminum wire
not evaluated in the development of these test methods.
to the nearest 0.001 g. Determine the mass/cm for the alumi-
6.4 Electric Muffle Furnace, capable of being maintained at num wire and cut a length of aluminum wire that is calculated
temperatures of 550 6 25°C and 925 6 25°C. The furnace to be slightly greater than 1.000 g. Trim off the excess wire
preferably having suitable apertures at front and rear to allow until the mass is 1.000 6 0.005 g. Dissolve the aluminum wire
a slow, natural draft of air to pass through. in 50 mL of concentrated hydrochloric acid. Heat gently. Cool
6.5 Electric Hot Plate, with or without magnetic stirring and transfer the solution to 1000 mL volumetric flask. Dilute to
capability. the mark with water.
6.6 Electric Oven, maintained at a temperature of 50 to 7.7.2 Silicon Standard Solutions—Obtain a ready made,
60°C. aqueous standard or prepare a standard from silicon dioxide.
6.7 Graduated Cylinders, 10, 25, 50, and 100 mL. 7.7.2.1 Silicon Solution (1000 mg/L)—Aqueous, ready
6.8 Pipettes, 1, 2, 5, 10, 20, and 25 mL. made commercial standard.
6.9 Platinum Dish, 100 mL capacity, cleaned with fused 7.7.2.2 Silicon Solution (1000 mg/L)—Using a zirconium
potassium hydrogen sulfate. crucible with a close fitting lid, fuse 2.140 6 0.0107 g of
6.10 Volumetric Flasks, 100 and 1000 mL. silicon dioxide (99.99 % purity) with 8 g of sodium hydroxide
6.11 All glassware must be carefully cleaned with 1 + 1 until a clear melt is obtained. Cool and dissolve the melt in
hydrochloric acid and rinsed thoroughly with water to mini- 100 mL of a solution of 1 part hydrochloric acid by volume and
mize contamination. The use of chromic acid cleaning solution 2 parts water by volume. Transfer this solution to a 1000 mL
is not recommended. volumetric flask and dilute to the mark with water. Immedi-
6.12 Zirconium crucible with close fitting zirconium lid, 30 ately, transfer the contents of the flask to a plastic bottle.
to 50 mL capacity. 7.8 Tartaric Acid/Hydrochloric Acid Solution—Dissolve 5 g
of tartaric acid in about 500 mL of water acidified with 40 mL
7. Reagents of concentrated hydrochloric acid and dilute to 1000 mL with
7.1 Purity of Reagents—Reagent grade chemicals shall be water.
used in all tests. Unless otherwise indicated, it is intended that 7.9 Toluene/2-Propanol Solution (1 + 1)—Mix one vol-
all reagents conform to the specifications of the Committee on ume of toluene with one volume of 2-propanol.
Analytical Reagents of the American Chemical Society where 7.10 Quality Control (QC) Samples, preferably are portions
such specifications are available.3 Other grades may be used, of one or more liquid petroleum materials that are stable and
provided it is first ascertained that the reagent is of sufficiently representative of the samples of interest. These QC samples
high purity to permit its use without lessening the accuracy of can be used to check the validity of the testing process as
the determination. described in Section 18.
7.2 Purity of Water—Unless otherwise indicated, reference
to water shall be understood to mean reagent water conforming 8. Quality Control (QC) Sample Preparation
to Type II of Specification D 1193. 8.1 Preparation of QC Samples shall follow the same
7.3 Flux—Mixture of 90 % lithium tetraborate and 10 % protocol as defined for the test specimen (Sections 9, 10, and
lithium fluoride. 11).
9. Sampling
3
Reagent Chemicals, American Chemical Society Specifications, American 9.1 The objective of sampling is to obtain a sample for
Chemical Society, Washington, DC. For suggestions on the testing of reagents not testing purposes that is representative of the entire quantity.
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Thus, take samples in accordance with the instructions in
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, Practice D 4057 or D 4177 . Typically, a gallon size container
MD. filled to approximately three-fourths of capacity is satisfactory.

2
 D 5184 – 01 (2006)
10. Sample Handling ensure transfer is complete. Make up to the mark with water.
10.1 Homogenization—It is extremely important to homog- Then, transfer the solution to a plastic bottle.
enize the fuel oil in the sample container in order to obtain a NOTE 6—Transferring the test solution to a plastic bottle is desirable
representative specimen. (Warning—Failure to use this ho- because the dilute acid solution contains fluoboric acid from dissolution of
mogenization procedure can invalidate the results because the flux. Storage tests have shown that there is no significant attack of
non-representative aliquots could be obtained and this could glassware in the short term (up to one week), and that the solution does not
lead to erroneous results.) contain fluoride ion above the 5 mg/L concentration.
10.2 Place the sample container in an oven at a temperature
12. Preparation of Calibration Solutions
of 50 to 60°C. Keep the container in the oven until the sample
comes to temperature. Insert the shaft of a high speed homog- 12.1 Blank Solution—Prepare a blank solution containing
enizer into the sample container so that the head of the shaft is only 0.4 g flux and 50 mL of the tartaric acid/hydrochloric acid
immersed to approximately 5 mm from the bottom of the solution diluted to 100 mL. Transfer it to a plastic bottle.
sample vessel. Mix the sample for about 5 min. 12.2 Aluminum—Prepare a 250 mg/L aluminum working
solution by diluting 25 mL of the 1000 mg/L standard solution
11. Specimen Preparation to 100 mL with water. To each of four clean 100 mL volumetric
flasks, add 0.4 g of flux and 50 mL of the tartaric acid/
11.1 Weigh a clean platinum dish to the nearest 0.1 g. hydrochloric acid solution. To successive flasks add 2, 4, 10,
Immediately transfer up to 50 g (but not less than 20 g) of the and 20 mL of the 250 mg/L aluminum working solution and
well-mixed sample, preferably containing about 1.3 mg alumi- dilute to 100 mL with water. The calibration solutions contain
num, to the platinum dish and re-weigh the dish and contents 5, 10, 25, and 50 mg/L of aluminum, respectively.
to the nearest 0.1 g to obtain the weight of the specimen. 12.3 Silicon—Prepare a 250 mg/L silicon working solution
NOTE 3—The specimen mass proposed, based on the aluminum content by diluting 25 mL of 1000 mg/L standard solution to 100 mL
will suffice for silicon as both elements are usually found in fuel oils at with water. To each of four clean 100 mL volumetric flasks,
similar concentrations. add 0.4 g of flux and 50 mL of the tartaric acid/hydrochloric
11.2 Warm the dish and contents gently with a bunsen flame acid solution. To successive flasks, add 2, 4, 10, and 20 mL of
until the sample can be ignited. Maintain the contents of the the 250 mg/L silicon working solution and dilute to 100 mL
basin at a temperature such that most of the combustible with water. These calibration solutions contain 5, 10, 25, and
material is removed and only carbon and ash remain. 50 mg/L of silicon, respectively.
12.4 Transfer all calibration standards to plastic bottles.
NOTE 4—If the specimen contains considerable amounts of moisture,
foaming and frothing can cause loss of material. If this is the case, discard NOTE 7—When both aluminum and silicon are being determined, the 5
the specimen and to a fresh portion add 1 to 2 mL of 2-propanol before to 50 mg/L calibration solutions can be combined providing there are no
heating. If this is not satisfactory, add 10 mL of a mixture of equal parts incompatibility problems caused by the reagents used in the preparation of
of toluene and 2-propanol and mix thoroughly. Place several strips of the standard solutions described in 7.7.1 and 7.7.2.
ashless filter paper in the mixture and warm gently. When the paper begins
to burn, the greater part of the water will have been removed. TEST METHOD A—INDUCTIVELY-COUPLED
PLASMA ATOMIC EMISSION SPECTROMETRY
11.3 Place the dish and contents in a muffle furnace main-
tained at a temperature of 550 6 25°C. Maintain the muffle
furnace at this temperature until all the carbon is removed and 13. Preparation of ICP Instrument
only ash remains. This may require more than 10 h in the 13.1 Instrument—Consult the manufacturer’s instructions
muffle furnace and may conveniently be done overnight. for the operation of the instrument. Design differences between
11.4 Cool the dish to room temperature, add 0.4 g of flux instruments, ICP excitation sources, and different selected
and mix with the ash. Place the dish in a muffle furnace analytical wavelengths for individual spectrometers make it
maintained at a temperature of 925 6 25°C for 5 min. Remove impractical to specify the required manipulations in detail.
the dish and ensure contact of the flux with the ash. Replace the 13.2 Peristaltic Pump—If using a peristaltic pump, inspect
dish in the muffle furnace and maintain at a temperature of the pump tubing and replace it, if necessary, before starting
925 6 25°C for 10 min. each day. Verify the solution uptake rate and adjust it to the
11.5 Remove the dish, cool the fusion melt to room tem- desired rate.
perature and add 50 mL of the tartaric acid/hydrochloric acid 13.3 ICP Excitation Source—Ignite the ICP excitation
solution. Place the dish and contents on the hot plate main- source at least 30 min before performing an analysis. During
tained at a temperature of approximately 80°C. Heat until the this warm-up period, nebulize water.
melt is dissolved. (Warning—Vaporization of a significant NOTE 8—Some manufacturers recommend even longer warmup peri-
amount of the liquid can lead to precipitation of an insoluble ods to minimize the variability of the measurements.
form of silica leading to erroneous results.)
13.4 Wavelength Profiling—Perform any wavelength profil-
NOTE 5—Prolonged heating can be necessary to dissolve the melt ing that may be called for in the normal operation of the
completely and obtain a solution. Agitation or the use of magnetic stirring instrument.
can be employed to speed dissolution of the melt.
13.5 Operation Parameters—Assign the appropriate oper-
11.6 Allow the solution to cool and then transfer it to a ating parameters to the instrument task file so that the desired
100-mL flask with water, washing the dish several times to elements can be determined. Parameters to be included are

3
 D 5184 – 01 (2006)
TABLE 1 Instrument Settings for Aluminum TABLE 2 Instrument Settings for Silicon
Wavelength, nm 309.3 Wavelength, nm 251.6
Fuel Acetylene Fuel Acetylene
Oxidant Nitrous oxide Oxidant Nitrous oxide
Lamp current As recommended by the manufacturer Lamp current As recommended by the manufacturer

Aspirate an aluminum standard (for example, 25 mg/L) into the

element, wavelength, background correction points (optional),
flame. Make adjustments to burner height, burner alignment,
interelement correction factors (optional), integration time and
acetylene flow rate, and impact bead to give maximum
three consecutive integrations.
absorbance (or minimum transmittance). Adjust the gain con-
14. ICP Calibration trol to set the maximum within the recommended working
14.1 Perform a five point calibration consisting of the blank region of the spectrometer.
and calibration standards at the beginning of analysis of each 16.3 Settings for Silicon Analysis:
batch of specimens. Use the check standard to determine if 16.3.1 Fit the silicon hollow cathode lamp, set the spectrom-
each element is in calibration. If the result obtained on the eter to the specified wavelength (see Table 2) and adjust the
check standard is outside 5 % of the expected value for any wavelength control to get maximum output.
element, make any adjustments to the instrument that may be 16.3.2 Follow a similar procedure to 16.2.2, aspirating a
necessary and repeat the calibration. silicon standard (for example, 25 mg/L) into the flame.
14.2 Alternatively, perform a two point calibration with the 17. Procedure
blank solution and most concentrated calibration standard. Use 17.1 AA Calibration and Test Specimen Analysis:
the check standard as described in 14.1. 17.1.1 The mode of calibration depends on the type of
15. Procedure readout facility on the atomic absorption spectrometer.
17.2 Calibration must be carried out prior to analysis of
15.1 ICP Analysis: each group of samples and after any change in instrumental
15.1.1 Specimen Analysis—Analyze the specimen solutions conditions because variations occur in the instrument behavior.
(see Section 11) in the same manner as the calibration Readings may also vary over short times from such causes as
standards (that is, same integration time, background correc- build-up of deposits on the burner slot or in the nebulizer. Thus,
tion points, plasma conditions, etc.). Rinse the plasma torch a single standard must be aspirated from time to time during a
between specimens by nebulizing water for 10 s. If the series of samples to check whether the calibration has changed.
concentrations of aluminum or silicon in the specimen solution The visual appearance of the flame is a useful check to detect
exceeds the calibration range, dilute the specimen solution with changes of condition.
the blank solution to bring it within the range of the calibration
standards. NOTE 9—A check after every fifth specimen is recommended.
15.2 Check Standard Analysis—Analyze the check standard 17.3 Spectrometers with Meter Readout:
after every fifth specimen. If the concentration of any element 17.3.1 Aspirate the calibration standards and blank solution
is outside 5 % of the nominal value, re-calibrate the instrument sequentially into the flame and record the meter readings.
and re-analyze the sample solutions back to the previous Aspirate the blank between each specimen.
acceptable check standard analysis. 17.3.2 If the spectrometer output is linear in absorbance,
15.3 Calculation and Report—See Section 18. plot a calibration curve of net absorbance (absorbance of a
calibration standard minus the absorbance of the blank) against
TEST METHOD B—FLAME ATOMIC ABSORPTION concentration. From this calibration curve, the concentration of
SPECTROMETRY aluminum or silicon in each specimen solution can be deter-
mined after similarly computing the net absorbance.
16. Preparation of AAS Instrument 17.3.3 If the spectrometer output is proportional to trans-
16.1 Instrument—Consult the manufacturer’s instructions mission, the net absorbance is given by:
for the operation of the atomic absorption instrument. Design
log ~d0!/~d1! (1)
differences between instruments make it impractical to specify
the required manipulations here. where:
16.1.1 Proper operating procedures are required for safety d0 = the meter reading due to the blank, and
as well as for reliability of results. An explosion can result from d1 = is the meter reading given by the standard or specimen
flame flash-back unless the correct burner head, gas flow rates solution.
and flame ignition/shutdown sequence are used. 17.4 Spectrometers With Digital Readout and Built-in (Non-
16.2 Settings for Aluminum Analysis: Microprocessor Controlled) Curvature Correction and Scale
16.2.1 Fit the aluminum hollow cathode lamp, set the Expansion Facilities:
spectrometer to the specified wavelength (see Table 1) and 17.4.1 Follow the manufacturer’s operating instructions.
adjust the wavelength control to get maximum output. Aspirate the appropriate calibration standards and blank solu-
16.2.2 Using the correct burner for nitrous oxide/acetylene, tion and set the digital readout to read directly in the required
and following the procedure specified in the manufacturer’s concentrations units carrying out a curvature correction pro-
operating instructions, ignite the nitrous oxide/acetylene flame. gram if necessary.

4
 D 5184 – 01 (2006)
TABLE 3 Repeatability TABLE 5 Reproducibility
A
Repeatability, mg/kg Reproducibility, mg/kgA
Element Range, mg/kg Element Range, mg/kg
ICP AAS ICP AAS
Al 7–139 0.0660 * X 0.2968 * X ** 2⁄3 Al 7–139 0.337 * X 0.7890 * X ** 2⁄3
Si 10–236 0.0643 * X 0.3539 * X ** 2⁄3 Si 10–236 0.332 * X 1.338 * X ** 2⁄3
A A
Where: X = mean concentration, mg/kg. Where: X = mean concentration, mg/kg.

TABLE 4 Calculated Repeatability (mg/kg) at Selected 19. Quality Control

Concentrations
ICP AAS
19.1 Confirm the performance of the test procedure by
Concentration, mg/kg analyzing a quality control (QC) sample (Section 15 for Test
Al Si Al Si
Method A or Section 16 for Test Method B).
5 0.3 0.3 0.9 1.0
10 0.7 0.6 1.4 1.7
19.1.1 When QC/Quality Assurance (QA) protocols are
20 1.3 1.3 2.2 2.6 already established in the testing facility, these may be used to
50 3.3 3.2 4.1 4.9 confirm the reliability of the test result.
100 6.6 6.4 6.5 7.7
250 ... 16 ... 14
19.1.2 When there is no QC/QA protocol established in the
testing facility, Appendix X1 can be used as the QC/QA
system.
17.4.2 Read the concentration of each specimen solution
20. Report
and blank directly from the concentration readout given by the
digital display from the spectrometer. 20.1 Report the results to the nearest 1 mg/kg as aluminum
17.5 Spectrometers With Digital Readout and Microproces- and silicon content by Test Method A or B.
sor Controlled Calibration Facilities:
21. Precision and Bias 4
17.5.1 Follow the manufacturer’s operating instructions,
aspirating the appropriate calibration standards and blank 21.1 Precision—The precision of these test methods was
solutions and using the recommended calibration program, to determined by statistical analysis of interlaboratory testing
obtain a direct readout in concentration units. results. In this study, eight laboratories analyzed nine different
17.5.2 The concentration of aluminum and silicon in each samples in duplicate.
specimen solution can thus be directly obtained after aspira- 21.1.1 Repeatability—The difference between two test re-
tion. sults, obtained by the same operator with the same apparatus
17.6 Analyze the specimen solutions in the same manner as under constant operating conditions on identical test material
the calibration standards. If the aluminum or silicon concen- would, in the long run, in the normal and correct operation of
trations in the specimen solutions exceed the calibration range, the test method, exceed the values in Table 3 and Table 4 only
dilute the specimen solution with the blank solution to bring it in one case in twenty.
into range of the calibration standards. 21.1.2 Reproducibility—The difference between two single
and independent results, obtained by different operators work-
18. Calculation ing in different laboratories on identical test materials, would in
18.1 Calculate the concentration in the sample according to the long run, in the normal and correct operation of the test
the following equations: method, exceed the values in Table 5 and Table 6 only in one
case in twenty.
aluminum, mg/kg 5 ~100 * C1 * d!/M (2)
21.2 Bias—The lack of suitable standard reference materi-
silicon, mg/kg 5 ~100 * C2 * d!/M (3) als precludes the determination of bias.
where: 22. Keywords
M = mass of sample taken in g,
d = dilution ratio, if required, and 22.1 AAS; aluminum; atomic-absorption-spectrometry;
C1, C2 = concentrations of aluminum and silicon (respec- emission-spectrometry; ICP; inductively-coupled-
tively) in mg/L as determined from either the read plasmaatomic-emission-spectrometry; fuel oils; silicon
out of the ICP instrument or the calibration curve
or direct readout of the atomic absorption instru- 4
Supporting data have been filed at ASTM International Headquarters and may
ment. be obtained by requesting Research Report RR: D02-1281.

5
 D 5184 – 01 (2006)
TABLE 6 Calculated Reproducibility (mg/kg) at Selected
Concentrations
ICP AAS
Concentration, mg/kg
Al Si Al Si
5 1.7 1.7 2.3 4.1
10 3.4 3.3 3.7 6.5
20 6.7 6.6 5.9 10
50 17 17 11 19
100 34 33 17 30
250 ... 83 ... 56

APPENDIX

(Nonmandatory Information)

X1. QUALITY CONTROL

X1.1 Confirm the performance of the instrument or the test test method, the frequency of QC testing is dependent on the
procedure by analyzing a quality control (QC) sample. criticality of the quality being measured, the demonstrated
stability of the testing process, and customer requirements.
X1.2 Prior to monitoring the measurement process, the user Generally, a QC sample is analyzed each testing day with
of the method needs to determine the average value and control routine samples. The QC frequency should be increased if a
limits of the QC sample (see Practice D 6299 and ASTM MNL large number of samples are routinely analyzed. However,
7).5 when it is demonstrated that the testing is under statistical
control, the QC testing frequency may be reduced. The QC
X1.3 Record the QC results and analyze by control charts sample precision should be checked against the ASTM method
or other statistically equivalent techniques to ascertain the precision to ensure data quality.
statistical control status of the total testing process (see Practice
D 6299 and ASTM MNL 7). Any out-of-control data should X1.5 It is recommended then, if possible, the type of QC
trigger investigation for root cause(s). The results of this sample that is regularly tested be representative of the material
investigation may, but not necessarily, result in instrument routinely analyzed. An ample supply of QC sample material
re-calibration. should be available for the intended period of use, and must be
homogenous and stable under the anticipated storage condi-
X1.4 In the absence of explicit requirements given in the tions.
X1.6 See Practice D 6299 or ASTM MNL 7, or a combina-
5
ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis, 6th ed., tion thereof, for further guidance on QC and Control Charting
available from ASTM Headquarters. techniques.

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