Verifikasi Metode Standar

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ASTM D 92 -12 b ASTM D 92 - 16 b
Pada point 11 Procedure
11.1 Manual Apparatus 11.1 Manual Apparatus
- Ditambahkan catatan :
Note 11-Initially the test cup may be filled below the filling mark to allow for thermal
expansion of the sample.
Analisa Flash Point

11.2 Automated Apparatus 11.2 Automated Apparatus

- Ditambahkan catatan :
Note 19-Initially the test cup may be filled below the filling mark to allow for thermal
expansion of the sample.

ASTM D 445 - 15a ASTM D 445 - 17a

Revisi Pada 3.2.1.2
Discuccion - PET is an acronym for portable electronic thermometers, a subset of
Discuccion - Portable electronic thermometers (PET) is an acronym sometimes digital contact thermometers (DCT)
used to refer to a subset of the devices covered by this definition.

Update pada point 17.1.1 , 17.2.1 dan 17.2.2

17.1.1 Determinability 17.1.1 Determinability

Based Oil at 40 °C10 0.0037 y (0.37%) Based Oil at 40 °C10 0.0037 y (0.37%)
Based Oil at 100 °C10 0.0036 y (0.36%) Based Oil at 100 °C10 0.0036 y (0.36%)
Formulated oils at 40 °C10 0.0037 y (0.37%) Formulated oils at 40 °C10 0.0037 y (0.37%)
Formulated oils at 100 °C10 0.0036 y (0.36%) Formulated oils at 100 °C10 0.0036 y (0.36%)
Formulated oils at 150 °C11 0.015y (1.5%) Formulated oils at 150 °C11 0.015y (1.5%)
Petroleum wax at 100 °C12 0.0080 y (0.80%) Petroleum wax at 100 °C12 0.0080 y (0.80%)
Residual fuel oils at 80 & 100 °C13 0.011 (y + 8) Residual fuel oils at 50 °C13 0.0244 y (2.44%)
Residual fuel oils at 50 °C13 0.017 y (1.7%) Residual fuel oils at 100 °C13 0.03 y (3%)
Additives at 100 °C14 0.00106 y1.1 Additives at 100 °C14 0.00106 y1.1
Gas oils at 40 °C15 0.0013 (y+1) Gas oils at 40 °C15 0.0013 (y+1)
Jet Fuels at -20 °C16 0.0018y (0.18%) Jet Fuels at -20 °C16 0.0018y (0.18%)
Kerosine, diesel fuels, biodiesel fuel blends at 40 °C17 0.0037 y (0.37%) Kerosine, diesel fuels, biodiesel fuel blends at 40 °C17 0.0037 y (0.37%)

17.2.1 Repeatability (r) 17.2.1 Repeatability (r)

Based Oil at 40 °C10 0.0101 x (1.01%) Based Oil at 40 °C10 0.0101 x (1.01%)
Based Oil at 100 °C10 0.0085 x (0.85%) Based Oil at 100 °C10 0.0085 x (0.85%)
Formulated oils at 40 °C10 0.0074 x (0.74%) Formulated oils at 40 °C10 0.0074 x (0.74%)
Formulated oils at 100 °C10 0.0084 x (0.84%) Formulated oils at 100 °C10 0.0084 x (0.84%)
Formulated oils at 150 °C11 0.0056 x (0.56%) Formulated oils at 150 °C11 0.0056 x (0.56%)
Petroleum wax at 100 °C12 0.0141 x1.2 Petroleum wax at 100 °C12 0.0141 x1.2
Residual fuel oils at 80 & 100 °C13 0.013 (x + 8) Residual fuel oils at 80 °C13 0.013 (x + 8)
Residual oils at 50 °C13 0.015 x (1.5%) Residual fuel oils at 100 °C13 0.08088 x (8.08%)
Additives at 100 °C14 0.00192x1.1 Residual oils at 50 °C13 0.07885 x (7.88%)
Gas oils at 40 °C15 0.0043 (x+1) Additives at 100 °C14 0.00192x1.1
Jet Fuels at -20 °C16 0.007 x (0.7%) Gas oils at 40 °C15 0.0043 (x+1)
Analisa Viscositas Kerosine, diesel fuels, biodiesel fuel blends at 40 °C17 0.0056 x (0.56%) Jet Fuels at -20 °C16 0.007 x (0.7%)
Kerosine, diesel fuels, biodiesel fuel blends at 40 °C17 0.0056 x (0.56%) Kerosine, diesel fuels, biodiesel fuel blends at 40 °C17 0.0056 x (0.56%)
Used (in-service) formulated oils at 40 °C18 0.000233 x1.722
Used (in-service) formulated oils at 100 °C18 0.001005 x1.4633

17.2.1 Reproducibility (R) 17.2.1 Reproducibility (R)

Based Oil at 40 °C10 0.0136 x (1.36%) Based Oil at 40 °C10 0.0136 x (1.36%)
Based Oil at 100 °C10 0.0190 x (1,90%) Based Oil at 100 °C10 0.0190 x (1,90%)
Formulated oils at 40 °C10 0.0122 x (1.22%) Formulated oils at 40 °C10 0.0122 x (1.22%)
Formulated oils at 100 °C10 0.0138 x (1.38%) Formulated oils at 100 °C10 0.0138 x (1.38%)
Formulated oils at 150 °C11 0.018 x (1.8%) Formulated oils at 150 °C11 0.018 x (1.8%)
Petroleum wax at 100 °C12 0.0366 x1.2 Petroleum wax at 100 °C12 0.0366 x1.2
Residual fuel oils at 80 & 100 °C13 0.04 (x + 8) Residual fuel oils at 80 °C13 0.04 (x + 8)
Residual fuel oils at 50 °C13 0.074 x (7.4%) Residual fuel oils at 100 °C13 0.1206 x (12.06%)
Additives at 100 °C14 0.00862x1.1 Residual oils at 50 °C13 0.08461 x (8.46%)
Gas oils at 40 °C15 0.0082 (x+1) Additives at 100 °C14 0.00862x1.1
Jet Fuels at -20 °C16 0.019 x (1.9%) Gas oils at 40 °C15 0.0082 (x+1)
Kerosine, diesel fuels, biodiesel fuel blends at 40 °C17 0.0224 x (2.24%) Jet Fuels at -20 °C16 0.019 x (1.9%)
Kerosine, diesel fuels, biodiesel fuel blends at 40 °C17 0.0224 x (2.24%)
Used (in-service) formulated oils at 40 °C18 0.000594 x1.722
Used (in-service) formulated oils at 100 °C18 0.003361 x1.4633

Dihapusnya point 17.3

The precision for used oils has not been determined but is expected to be poorer
than that for formulated oils. Because of the extreme variability of such used oils, -
it is not anticipated that the precision of used oils will be determined.

Revisi pada point 13.2

If periodic verification of the viscometer calibration using certified viscosity reference
standards (see 9.2) is outside of the accpetable tolerance band, the viscometer may
- need to be cleaned.

Revisi pada point 12

Procedure for opaque liquids Procedure for residual fuel oils and opaque liquids

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ASTM D 473 - 07 ASTM D 473 - 07 (Reapproved 2017) e1
Revisi pada point 1.2
Analisa Sedimen The values given in parenthese are information only. No other units of measurement are included in this standard.

ASTM D 95-05 ASTM D 95-13e1

2. Referenced Document
- Penambahan metode standar pada 2.1 ASTM Standard :
ASTM D 235 Specification for mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry
Cleaning Solvent)

Pada point 6. Solvent-Carrier Liquid

Ditambahkan Note :
Note 3- Examples of suitable solvents include Types I and IV and classes A and B of
- specification D 235

Note 4- It is recommended to use a wide boiling range solvent with 10% boiling
- below 100 °C to help to ensure an even distillation rate.

Pada point 6 Solvent-Carrier Liquid

Diupdate pada point 6.1 , 6,1.2 dan table 1
Analisa Kadar Air

6.1 A water-immiscible solvent-carrier liquid that is miscible in the material being

tested (see Table I) shall be used.

6.1.2 Petroleum Distillate Solvent-A petroleum distillate solvent containing at least

2% (V/V) aromatics and with 100 an initial boiling point (IBP) greater than 80 °C (176
°F); and a final boiling point (FBP) below 250 °C (482 °F) shall be used.

Table I Type of Solvent-Carrier Liquid to Use Versus Material to Be Tested Table I Type of Solvent-Carrier Liquid to Use Versus Material to Be Tested

Type of Solvent-Carrier Liquid : Material to Be Tested Type of Solvent-Carrier Liquid : Material to Be Tested
Aromatic : Asphalt, bitumen, tar, and related products Aromatic : Asphalt, bitumen, tar, and related products
Volatile Spirits : Greases Petroleum Distillate : Fuel oil, lubricating oil additivies
Volatile Spirits : Greases

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ASTM D 1298 - 05 ASTM D 1298-12b
Penambahan pada point 1. Scope yaitu :

1.2 The initial hydrometer readings obtained are uncorected hydrometer readings
and not density measurements.Reading are measured on a hydrometer at either the
reference temperature or at another convenient temperature, and readings are
corrected for the meniscus effect, the thermal glass expansion effect, alternative
calibration temperature effects and to the reference temperature by means of the
Petroleum Measurement Tables; values obtained at other than the reference
temperature being hydrometer readings and not density measurements.

1.3 Reading deternined as density, relative density, or API gravity can be converted
to equivalent values in the other units or alternative reference temperatures by
means of Interconversion Procedures (API MPMS Chapter 11.5), or Adjunct to D1250
Guide for Petroleum Measurement Tables (API MPMS Chapter 11.1), or both, or
tables, as applicable.

1.4 The initial hydrometer readings determined in the laboratory shall be recorded
before performing any calculations. The calculations required in Section 10 shall be
applied to the initial hydrometer reading with observations and result reported as
required by Section 11 prior to use in a subsequent calculation procedure (ticket
calculation, meter factor calculation, or base prover volume determination)

1.6 The values stated in SI units are to be regarded as standard.

1.6.1 Exception-The values given in parentheses are provide for information only.

1.8 This international standard was developed in accordance with internatinally

recognized principles on standardization established in the Decision on Principles for
Analisa Density the Development of International Standards, Guide and Recomendations issued by
the World Trade Organization Technical Barriers to Trade (TBT) Commitee.

Penambahan pada point 2 Referenced Documents.

2.2 API Standards

MPMS Chapter 11.1 Temperature and Pressure Volume Correction Factors for
Generalized Crude Oils, Refined Products and Lubricating Oils (Adjunct to ASTM
D1250)
MPMS Chapter 11.5 Density/Weight/Volume Intraconversion

2.5 ASTM Adjuncts

Adjunct to D1250 Guide for Petroleum Measurement Tables (API MPMS Chapter
11.1)

Penambahan pada point 3. Therminology

3.1.4 Hydrometer reading, n-the point on the hydrometer scale at which the surface
of the liquid cuts the scale.

3.1.4.1 Discussion-In practice for transparent fluid this can be readily determined by
aligning the surface of the liquid on both sides of the hydrometer and reading the
Hydrometer scale where these surface readings cut the scale (Hydrometer Reading-
Observed). For nontransparent fluids the point at which the liquid surface cuts
Hydrometer scale cannot be determined directly and requires a correction (Meniscus
Correction). The values represented by the point (Meniscus Reading) at which the
liquid sample rises above the main surface of the liquid subtracted from the values
represented by where the main surface of the liquid cuts the Hydrometer scale is the
amount of the correction or Meniscus correction. This meniscus correction is
documented and then subtracted from the value represented by the Meniscus
Reading to yield the Hydrometer Reading corrected for the Meniscus (Hydrometer
Reading - Observed, Meniscus Corrected)

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Penambahan pada point 4. Summary of Test Method

4.1 The appropriate hydrometer , also at a similiar temperature, are lowered into 4.1 The appropriate hydrometer and thermometer, also at a similiar temperature,
the test portion and allowed to settle. are lowered into the test portion and allowed to settle.
The observed hydrometer reading is corrected for the meniscus effect, the thermal
glass expansion effect alternative calibration temperature effects and then reduced
to the reference temperature by means of the volume correction factors or tables as
applicable by use of the appropriate Adjunct to D1250 Guide for Petroleum
Measurement Tables (API MPMS Chapter 11.1) and observed temperature from the
thermometer.

4.2 If necessary, the hydrometer cylinder and its contents are placed in a constant
temperature bath to avoid excessive temperature variation during the test.

Revisi pada point 5. Significant and Use

5.1 at standard reference temperatures of 15 °C or 60 °F during custody transfer

5.2 Additionally for both transparent and opaque fluids the readings shall be
corrected for the thermal glass expansion effect and alternative calibration
temperature effects before correcting to the reference temperature.

Analisa Density Revisi pada point 6. Appartus

6.1.1 The instrument is classedas certified and the appropriate corrections for the
meniscus effect, the thermal glass expansion effect, and alternative calibration
temperature effects shall be applied to the observed readings prior to the
corrections.

6.2.1 The stated repeatability and reproducibility values are not applicable if
alternative fluids are used in the liquid-in-glass thermometers.

Penambahan pada point 7.Sampling

7.3.2 Waxy Crude Petroleum-If the petroleum has an expected pour point above 10
°C, or a cloud point or WAT above 15 °C, warm the sample to a temperature that is
sufficient for ensuring the material is fluid enough to provide adequate mixing
without excessively heating the material that would otherwise compromise the
integrity of the sample. Samples heated to 9 °C above its pour point, or 3 °C above its
cloud point or WAT have been found to be suitable temperatures to warm samples
prior to mixing.

7.3.3 Waxy Distillate-Warm the sample to a temperature that is sufficient for

ensuring the material is fluid enought to provide adequate mixing without
excessively heating the material that would otherwise compromise the integrity of
the sample. Samples heated to 3 °C above its cloud point or WAT have been found to
be suitable temperatures to warm samples prior to mixing.

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ASTM E 1621 - 05 ASTM E 1621-13
Revisi dan penambahan pada bagian 1. Scope

1.1 This guide covers guidelines for developing and describing analytical
procedures using wavelenght dispersive X-Ray spectrometer.
1.1 This guide provides guidelines for developing and describing analytical
procedures using wavelenght dispersive X-Ray spectrometer for elemental analysis
of solid metals, ores, and related materials. Material forms discussed herein include
solids, powders, and solid forms prepared by chemical and physical processes such
as borate fusion and pressing of briquettes.

- 1.2 Liquids are not discussed in this guide because they are much less frequently
encountered in metals and mining laboratories. However,aqueous liquids can be
processed by borate fusion to create solids specimens, and X-Ray spectrometers can
be equipped to handle liquids directly.

- 1.3 Some provisions of this guide may be applicable to the use of an energy
dispersive X-Ray spectrometer.

Revisi pada bagian 2. Referenced Documents

2.1 ASTM Standards:
ASTM E 305 Practice for Establishing and Controlling Atomic Emission Dihapusnya ASTM E 305 Practice for Establishing and Controlling Atomic Emission
Spectrochemical Analytical Curves Spectrochemical Analytical Curves

Penambahan E.2857 Guide for Validating Analytical Methods

Revisi pada bagian 4. Summary of Guide

- 4.1 Important aspects of test equipment for wavelenght dispersive X-ray

fluorescence spectrometry are discussed including equipment components and
accessories, reagent, and materials. Key aspects of the application of X-Ray
spectrometry to materials analysis are discussed including interferences and
correction options, specimen preparation by a variety of procedures, and materials
and accesories for presentation of specimens for measurement in spectrometers.
Key elements of measurement procedures, calibrations procedures, and result
reporting are explained.

4.2 The test specimen is prepared with a clean, uniform,flat surface. It may be
prepared by grinding, polishing, or lathing a metal surface or by fusing or
briquetting a powder. This surface is irradiated with a primary sourceof X-Rays.
Analisa Alumunium
The secondary X-Rays produced in the specimen are dispersed according to their
wavelenght by means of crystals or synthetic multilayers. Their intensities are
measured by suitable detector at selected wavelenghts and converted to count
by detector. COncentrstions of the elements are determined from the measured
intensities of analyte X-Ray line using analytical curves prepared with suitable
reference materials. Either a fixed multi-chanel simultaneous system or a
sequential monochromator system may be used to provide determinations of the
elements.
4.2 In an X-ray spectrometric test method, the test specimen is prepared with a
clean, uniform,flat surface. It may be prepared by grinding, polishing, or lathing a
metal surface or by fusing or briquetting a powder. This surface is irradiated with a
primary sourceof X-Rays. The secondary X-Rays produced in the specimen are
dispersed according to their wavelenght by means of crystals or synthetic
multilayers. Their count rates at selected wavelenght , hereinafter called intensities,
are measured by suitable detector systems. Amount of the elements are determined
from the measured intensities using analytical curves prepared with suitable
calibrants.

- 4.3 Important aspects of background estimation are covered in an appendix to the

guide.

Revisi pada bagian 5. Significance and Use

5.1 X-Ray fluorescence spectrometry can provide an accurate and precise
determination of metallic and many non-metallic elements. This guide covers the
information that should be included in an X-Ray spectrometric analytical method
and provides direction to the analyst for determining the optimum conditions
needed to achieve acceptable accuracy.
5.1 X-Ray fluorescence spectrometry can provide an accurate and precise
determination of metallic and many non-metallic elements in a wide variety of solid
and liquid materials. This guide covers the information that should be included in an
X-Ray spectrometric analytical method and provides direction to the analyst for
determining the optimum conditions needed to achieve acceptable accuracy.

5.2 The accuracy of an analysa is a function of the calibration scheme, the sample 5.2 The accuracy of determination is a function of the calibration scheme, the sample
preparation, and the sample homogeneity. Close attention to all aspects of these preparation, and the sample homogeneity. Close attention to all aspects of these
areas is necessary to achieve the best results. areas is necessary to achieve acceptable results.

- 5.3 All concepts discussed in this guide are explored in detail in a number of
published texts and in the scientific literature.

Revisi pada bagian 6. Interferences

6.1 Line overlaps, either total or partial, may occur for some elements.
Fundamental parameter equations require that the net intensities be free from
line overlap effects. Some empirical scheme incorporate line overlap corrections
in their equations. If sufficient sensitivity exists, it may be possible to reduce or
eliminate the overlap by choosing a higher level of collimation in the secondary X-
Ray path from specimen to dispersive element or detector. See Appendix X1 for
opttional approaches to the correction of line overlap effects.
6.1 Line overlaps, either total or partial, may occur for some elements. If sufficient
sensitivity exists, it may be possible to reduce or eliminate the overlap by choosing a
higher level of collimation in the secondary X-Ray path from specimen to dispersive
element or detector. See Appendix X1 for opttional approaches to the correction of
line overlap effects.

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- 6.1.1 Fundamental Parameter (FP) equations require the the net intensities with line
overlaps and beckground subtraction performed before the FP calculations are
cerried out. Some empirical schemes incorporate line overlap corrections in their
equations, and some software allows combinations of empirical and FP calculations
chosen by element or other analyte.

- 6.1.2 Additionally, line overlap interferences may occur from characteristic line
generated from the target material of the X-Ray tube and scattered from the
specimen either inelastically (known as Compton scatter) or elastically (known as
Rayleigh scatter). These may be reduce or eliminated by the use of primary beam
filters, with a consequent loss os sensitivity.

6.2 Interelement effects or matrix effects may exist for some elements. An
empirical way to compensate for these effects is to prepare a series of calibration
curves that cover the designated concentration ranges to be analyzed. a Large
suite of carefully designed reference materials is necessary for this approach. A
series of samples in which all elements are relatively constant, except for the
analyte, is necessary, if the analyte is subject to large effects from some other
element in the matrix. The composition of the specimen being analyzed must
match closely the compsition of the reference material used to prepare the
particular calibration curves
6.2 Interelement effects (sometimes called matrix effects, see Note 1) may be
significant for some elements. An empirical way to compensate for these effects is to
prepare a series of calibration curves that cover the designated concentration ranges
to be analyzed. a Large suite of carefully designed reference materials is necessary
for this approach. A series of samples in which all elements are relatively constant,
except for the analyte, is necessary, if the analyte is subject to large effects from
some other element in the matrix. Typically, more accurate result are obtained when
the compositions of the calibrants used to prepare the particular calibration curves
are similar to the compositions of materials being analyzed.

Note 1-Interelement effects are not interferences in the spectrometric sense, but Note 1-Interelement effects are not interferences in the spectrometric sense, but will
will contribute to errors in the analysis if not properly addressed. contribute to errors in the analysis if not properly addressed. Interelement effects
result from the absorption of X-Rays to differing extents by the atoms in the
specimen according to the mass absorption coefficient.

6.3 Errors From Metallurgical Structure- The intensity for titanium is higher in this
6.3 Errors From Metallurgical Structure- The intensity for titanium is higher in this sample than it would be if the titanium, niobium, carbon, and iron were always in
sample than it would be if the titanium were in solid solution. solid solution.

Revisi pada point 7. Appartus

7.1.1.3 Grinding belts or disks shall be changed at regular, specified intervals in
order that changes in abrasive grit due to repeated use do not affect the
repeatability of the roughness of the sample finish. This is particularly important
in alloys which exhibit smearing of a softer component over the sample matrix.
Analisa Alumunium
7.1.1.3 Grinding belts or disks shall be changed at regular, specified intervals because
abrasives lose their ability to remove material efficiently and without inducing
contamination. This is particularly important in alloys that exhibit smearing of a
softer component cross the surface.

- 7.1.1.4 Provision of flowing water across the surface of a grinding wheel cools the
specimen and removes debris. Chemical coolants , such as those used in machine
shops, should not be used, except for special purposes.

- 7.1.1.5 The use of lathe, or similar type of machine, is recommended for soft metals
or metals that have components that can smear when surfaced with an abrasive
disk. The feed on the cutting tools should be constant, automatically controlled, to
give a consistent finish.

7.2.1 Jaw Crusher or steel mortal and pestle , for initial crushing of lump. 7.2.1 Jaw Crusher or steel mortal and pestle , for initial crushing of large chunks of
material.

7.2.2 Plate grinder or pulverizer with one static and one rotating disk for futher 7.2.2 Plate grinder or pulverizer with one static and one rotating disk for futher
grinding . grinding or crushing.

7.2.3 Rotary disk mill or shatterbox , with hardened grinding containers and timer 7.2.3 Rotary disk mill or swing mill, with hardened grinding containers and timer
control for final grinding. control for final grinding.

7.2.5 Fusion equipment, with timer capable of heating the sample and flux to at 7.2.5 Fusion equipment, with timer capable of heating the sample and flux to at least
least 1000 °C and homogenizing the melt. 975 °C and homogenizing the melt.

7.2.6.1 Vitreous Carbon 20 mL to 30 mL capacity with flat bottom 30 mm to 35 mm in

7.2.6.1 Vitreous Carbon 20 mL capacity with flat bottom to 35 mm in diameter. diameter.

7.2.6.2 95% Platinum/ 5% Gold alloy with 30 mL capacity 7.2.6.2 95% Platinum/ 5% Gold alloy with 30 mL to 35 mL capacity

7.2.7 Platinum/Gold Casting Mold (95%/ 5%) 30 - 35 mL capacity, with flat bottom
30 - 40 mm in diameter. 7.2.7 Platinum/Gold Casting Mold (95%/ 5%) having a flat , optical-polished bottom
and sufficient capacity to hold the quantity of glass needed to make a cast bead of
roughly uniform thickness across the entire diameter, typically 30 mm to 40 mm.

7.2.8 Polishing Wheel suitable for polishing the fused button to obtain a flat 7.2.8 Polishing Wheel suitable for polishing the fused button to obtain a flat uniform
uniform surface for irraditaion. surface for irraditaion. For machines that cast a bead in a polished dish, this step
may not be necessary.

- 7.3.1 X-Ray Tubes, with targets of various high-purity elements that are capable of
continuous operation at potentials and currents that will excite the elements to be
determined.

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7.3.3 X-Ray Tubes, with target of various high-purity elements, that are capable of 7.3.3 The instrument may be equipped with an external line voltage regulator or a
continuous operation at potentials and currents that will excite the elements to transient voltage suppressor.
be determined.
8.1 Purity of reagents - All reagents used in this test method shall conform to the 8.1 Purity of reagents - Reagents used in X-Ray fluorescence test methods must. Be
"Reagent Grade" specifications of the American Chemical Society. Be evaluated
for appropriate purity for the stated purpose and the expected performance of
the test method.
8.2 Binder - Sodium tetraborate (Na2Ba4O7), polyethylene glycol, fibrous
cellulose, or spectrographic grade graphite (200 mesh , briquetting type).
8.3 Detector Gas (P-10), consisting of a mixture of 90% argon and 10% methane,
for use with gas-flow proportional counters. Other gases are used to enchance
sensitivity over selected wavelength ranges.
8.4 Fluxes - Sodium tetraborate (Na2B4O7), fused and dried; lithium tetraborate
(Li2B4O7), Lithium metaborate (LiBO2) or lithium , mixtures of tetraborate and
metaborate, boric anhydrate (B2O3) .
9.1 Certified Reference Materials are avaiilable from the National Institute of
Standards and Technology and other certification ageneies.
9.2 Reference Materials with compositions similar to that of the test specimen
Analisa Alumunium and containing varying amounts of the elements to be determined may be used
provided they have been previously analyzed in accordance with ASTM test
methods. These reference materials should be homogeneuous and free of voids
or porosity.
10.1 Occupational Health and Safety Standards for ionizing shall be observed at
all X-Ray emission spectrometer installations. Operating and maintenance
personnel shall follow the guidelines of safe operating procedures given in
current handbooks and publications from the National Institute of Standards and
Technology, the U.S Goverment Printting Office or similar handbooks or radiation
safety as well as specific state regulations.
10.2 Monitoring Devices, either film badges or dosimeters may be worn by all
operating and maintenance personnel. Safety pracftice shall conform to
applieable local, state, and federal regulations. To meet local, state, and federal scattered radiation may be required by governing laws or regulations.
radiation standards, periodic radiation surveys of the equipment for leaks and
excessive scattered radiation shall be made by a qualified person using an
ionization chamber detector. The personal film badge survey record, the
radiation survey record, and an equipment maintennace record shall be available
upon request.
11.2 Metal Samples - Prepare the reference materials and test specimens to
provide has a clean, flat uniform surface to be exposed to the X-Ray beam. For
abrasive sanding, select a grit size and use it exclusively for all reference materials
and test specimens. See 7.1.1.2 and 7.1.1.3 Refinish the surface of the reference
materials and test specimens as needed to eliminate oxidation before
measurement.
Page 7 of 8
Metode Versi Baru
Revisi pada point 8. Reagents and Materials
evaluated for appropriate purity for the stated purpose and the expected
performance of the test method.
8.2 Binders - One of wide variety of compounds or materials that provide cohesion of
particles in a briquette including polyethylene glycol, cellulose, spectrographic grade
graphite (< 74 mikro meter briquetting type), borate compounds, and other
chemicals.
8.3 Detector Gas, typical detector gas consists of a mixture of 90% argon and 10%
methane, for use with gas-flow proportional counters. Other gases are used to
enchance sensitivity over selected wavelength ranges.
8.4 Fluxes - Lithium tetraborate (Li2B4O7), Lithium metaborate (LiBO2), mixtures of
tetraborate and metaborate, boric anhydrate (B2O3) and sodium tetraborate
(Na2B4O7). Prefused versions of the borate fluxes are available in high-purity
versions, some of which are mixed with halide compound non-wetting agents,
fluidizers, and heavy absorbers, for example, lanthanum oxide. There may be
additional flux composition suitable for dissolution of samples.
Revisi pada point 9. Reference Materials
9.1 Certified Reference Materials are avaiilable from the National Institute of
Standards and Technology from other national metrology institutes, and from other
private and public organizations that certify reference materials for chemical
composition in accordance with a relevant quality system incorporating standards
and guides from the International Organization for Standardization (ISO) and with
relevant supplemental standards and guidelines implemented by standards
development organizations concerned with a particular business sector.
9.2 Reference Materials with matrix compositions similar to that of the test
specimen and containing varying amounts of the elements to be determined may be
used provided they have analyzed in accordance with validated test methods. These
reference materials should be sufficiently homogeneous for the intended purpose.
Revisi pada point 10. Hazards
10.1 Exposure to excessive quantities of high energy radiation such as those
produced by X-Ray spectrometers is injurious to health. The operator should take
appropriate actions to avoid exposing any part of their body to primary X-Rays ,
secondary and scattered X-Radiation that may be present. The X-ray spectrometer
should be operated in accordance with regulations governing the use of ionizing
radiation. Manufacturers of X-Rays fluorescence spectrometers typically build
appropriate shielding and safety interlocks into X-Ray equipment during
manufacturing, which minimize the risk of excessive radiation exposure to operators.
Operators should not attempt to bypass or defeat safety devices. Only authorized
personnel should service X-Ray spectrometers.
10.2 Monitoring Devices, such as film badges or dosimeters may be used by operator
and maintainers. Periodic radiation surveys of the equipment for leaks and excessive
Revisi pada point 11. Preparation of Reference Materials and Test Speciments
11.2 Solid Metal Samples - Prepare the reference materials and test specimens so
that each has a clean, flat uniform surface to be exposed to the X-Ray beam. For
abrasive sanding, select a final grit size and use it exclusively for all reference
materials and test specimens. Several coarser grits may be needed before the final
grit can be used. Choosen the final grit small enough to minimize the effects of
grinding striations on measured intensity. See Note 2 and 7.1 . Refinish the surface of
the reference materials and test specimens using the same batches of all grit papers
on al specimens, even if some samples were previously finished with the same grit,
but of a differen batch.
 Verifikasi Metode Standar
Metode Metode Versi Lama
- Note 2- The final grit size should be small enought to minimize shadowing effects in
11.3 Nonmetallic Samples - Dry the material. Then reduce it both in particle size
and quantity, by crushing and pulverizing integrated with splitting or riffling,
ending with approximately 100 g of material that has a particle size of less than
200 mesh (74 mikrometer) .
11.3.1 Briquettes - Mix the sample with a suitable binder. (See 8.2). Ratios of 10 g
+ 1 g to 20 g + 1 g of sample + 1 binder are common. Grind and blend the sample
and binder for a fixed time (generally 4 min in a disk mill). Press the sample -
Analisa Alumunium binder mixture into a briquette using a fixed pressure of 140 to 550 MPa (20000
to 80000 psi) and maintaining the pressure for a minimum of 10 s before
releasing the briquette. Holding the pressure at 140 MPa (20000 psi) for about 10
s before increasing it to maximum allows air to escape from the mixture and
reduces the possibility of the briquette bursting from internal pressure.
11.3.2 Fused Beads-Use a predermined mix of sample to flux combination. A 0.3 g
of sample to 0.5 g of sodium tetraborate or 1,0 g of sample to 4,0 g to 10,0 g of
lithium tetraborate fluxes are commonly used mixtures . Mix weighed amounts of
sample and flux and place the mixture in clean platinum/gold or vitreous carbon
crucible. Heat at a fixed temperature, ussually from 950 C to 1100 C, until
thoroughly melted. Swirl the crucible several times to ensure a homogeneous
fusion and to remove particles from the crucible walls. Fusion time may vary from
2 min to 10 min, depending on the sample, flux, and to sample to flux ratio.
(Warning - ensure the sample is completely oxidized prior to fusing with the flux.
Un-oxidized metals may alloy with the platinum/gold crucible and destroy it)
Menyetujui,
Patan Ikhsan
Supt QC Chem Lab & BF Complex
Page 8 of 8
Metode Versi Baru
which X-Rays are absorbed by the raised portions of metal on either side of the
grooves created by grinding. To check for problems, place a prepared specimen in
the X-Ray spectrometer with the grinding marks paralled to the optical path and with
spinning disabled. Measure the intensities of all elements. Then, move the specimen
so the grinding marks are perpendicular to the optical path and measure again. If the
intensities of any elements decrease significantly, there is grinding-included
absorption. During measurements, spinning of all specimens may prevent the effects
from causing biases.
11.3 Nonmetallic Samples - Dry the material. Then reduce it both in particle size and
quantity, by crushing and pulverizing followed by splitting or riffling, ending with
approximately 100 g of material that has a particle size distribution with a maximum
of 74 mikrometer (200 mesh).
11.3.1 Briquettes - Mix the sample with a suitable binder. (See 8.2). Ratios of 10 g + 1
g to 20 g + 1 g of sample + 1 binder are common. Grind and blend the sample and
binder for a fixed time (generally 2 min to 4 min in a disk mill). Press the sample -
binder mixture into a briquette using a fixed pressure of 140 MPa to 550 MPa (20000
psi to 80000 psi) and maintaining the pressure for a minimum of 10 s before
releasing the briquette. Holding the pressure at 140 MPa (20000 psi) for about 10 s
before increasing it to maximum or pumping a vacuum on the side port of a die set
allows air to escape from the mixture and reduces the possibility of the briquette
bursting from internal pressure.
11.3.2 Fused Beads-Use a predermined mix of sample to flux combination. Develop
and apply a fusion procedure that is appropriate for the matrix and elements of
interest. Automated fusion equipment is readily available from several suppliers. For
example, a 1,0 g of sample plus 4,0 g to 10,0 g of mixed lithium borate fluxes are
commonly used. Mix weighed amounts of sample and flux and place the mixture in
clean platinum/gold or vitreous carbon crucible. Heat at a fixed temperature,
ussually from 950 C to 1100 C, until thoroughly melted. Mix the crucible several
times to ensure a homogeneous fusion and to remove particles from the crucible
walls. Fusion time may vary from 2 min to 10 min, depending on the sample, flux,
and to sample to flux ratio. (Warning - ensure the sample is completely oxidized
prior to fusing with the flux. Un-oxidized metals may alloy with the platinum/gold
crucible and destroy it)
Memverifikasi,
Maya Aurelia A
Plt. Engineer