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ASTM D6069-96

(Test Method)

Standard Test Method for Trace Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure Chemiluminescence Detection

Standard Test Method for Trace Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure Chemiluminescence Detection

SCOPE
1.1 This test method covers the determination of total nitrogen (organic and inorganic) in aromatic hydrocarbons, their derivatives and related chemicals.  
1.2 This test method is applicable for samples containing nitrogen from 0.2 to 2 mgN/kg. For higher nitrogen concentrations refer to Test Method D4629.  
1.2.1 The detector response of this technique within the specified scope of this test method is linear with nitrogen concentration.  
1.3 The following applies to all specified limits in this test method: for purposes of determining conformance with this test method, an observed value or a calculated value shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit , in accordance with the rounding-off method of Practice E29.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 9.

General Information

Status
Historical
Publication Date
09-Jun-2001
ICS
71.040.40 - Chemical analysis
Technical Committee
D16 - Aromatic, Industrial, Specialty and Related Chemicals
Drafting Committee
D16.04 - Instrumental Analysis
Current Stage
Ref Project

Relations

Replaced By
ASTM D6069-01 - Standard Test Method for Trace Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure Chemiluminescence Detection
Effective Date
10-Jun-2001

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ASTM D6069-96 - Standard Test Method for Trace Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure Chemiluminescence DetectionASTM D6069-96 - Standard Test Method for Trace Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure Chemiluminescence Detection
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ASTM D6069-96 - Standard Test Method for Trace Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure Chemiluminescence Detection
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NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn. Contact ASTM International (www.astm.org) for the latest information.
Designation: D 6069 – 96
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
Trace Nitrogen in Aromatic Hydrocarbons by Oxidative
Combustion and Reduced Pressure Chemiluminescence
1
Detection
This standard is issued under the fixed designation D 6069; 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 2.2 Other Documents:
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
1.1 This test method covers the determination of total
5
1910.1200
nitrogen (organic and inorganic) in aromatic hydrocarbons,
their derivatives and related chemicals.
3. Terminology
1.2 This test method is applicable for samples containing
3.1 Definitions:
nitrogen from 0.2 to 2 mgN/kg. For higher nitrogen concen-
3.1.1 reduced pressure chemiluminescence—a chemical re-
trations refer to Test Method D 4629.
action at pressure less than 760 mm mercury (Hg) in which
1.2.1 The detector response of this technique within the
light is emitted.
specified scope of this test method is linear with nitrogen
3.1.2 oxidative pyrolysis—a process in which a sample
concentration.
under goes combustion in an oxygen rich environment at
1.3 The following applies to all specified limits in this test
temperatures greater than of 650°C.
method: for purposes of determining conformance with this
3.1.2.1 Discussion—Organic compounds pyrolytically de-
test method, an observed value or a calculated value shall be
compose to carbon dioxide, water and elemental oxides.
rounded off “to the nearest unit” in the last right-hand digit
used in expressing the specification limit, in accordance with
4. Summary of Test Method
the rounding-off method of Practice E 29.
4.1 A specimen is introduced into a gas stream, at a
1.4 This standard does not purport to address all of the
controlled rate, and carried into a high temperature furnace
safety concerns, if any, associated with its use. It is the
(>900°C) where an excess of oxygen is added. Pyrolysis
responsibility of the user of this standard to establish appro-
converts organic material in the specimen to carbon dioxide
priate safety and health practices and determine the applica-
and water. Organic nitrogen and inorganic nitrogen com-
bility of regulatory limitations prior to use. For specific hazard
pounds, present in the specimen, are converted to nitric oxide
statements, see Section 9.
(NO). Nitric oxide reacts with ozone in the detector producing
nitrogen dioxide molecules in an excited state. As the excited
2. Referenced Documents
nitrogen dioxide molecules relax to ground state, light is
2.1 ASTM Standards:
emitted. This light is detected by a photomultiplier tube with
D 1555 Test Method for Calculation of Volume and Weight
2
the resulting signal proportional to the concentration of nitro-
of Industrial Aromatic Hydrocarbons
gen in the sample. Operating the detector at a reduced pressure,
D 3437 Practice for Sampling and Handling Liquid Cyclic
2 lowers the probability of the excited nitrogen dioxide mol-
Products
ecules colliding with other molecules before it under goes
D 4629 Test Method for Organically Bound Trace Nitrogen
chemiluminescence. Thus, reduced pressure provides im-
in Liquid Petroleum Hydrocarbons By Syringe/Inlet Oxi-
3 proved sensitivity and lower noise.
dative Combustion and Chemiluminescence Detection
E 29 Practice for Using Significant Digits in Test Data to
5. Significance and Use
4
Determine Conformance with Specifications
5.1 This method has been prepared to detect and quantitate
E 691 Practice for Conducting an Interlaboratory Study to
nitrogen-containing compounds such as N-formylmorpholine
4
Determine the Precision of a Test Method
(4-formylmorpholine, Chemical Abstract Service numbers
(CAS) No. 250-37-6) or 1-methyl-2-pyrrolidinone (NMP)
1
This test method is under the jurisdiction of ASTM Committee D-16 on
(CAS) No. 872-50-42 at a concentration of 1.0 mgN/kg or less
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
in aromatic hydrocarbons used or produced in manufacturing
Subcommittee D16.0E on Instrumental Analysis.
Current edition approved Dec. 10, 1996. Published February 1997.
2
Annual Book of ASTM Standards, Vol 06.04.
3 5
Annual Book of ASTM Standards, Vol 05.02. Available from the Superintendent of Documents, U.S. Government Printing
4
Annual Book of ASTM Standards, Vol 14.02. Office, Washington, DC 20402.
1

---------------------- Page: 1 ----------------------
D 6069
processes. These nitrogen-containing compounds a
...

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1.1 This test method covers the determination of organic chloride in aromatic hydrocarbons, their derivatives, and related chemicals.  
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1.5 Organic chloride values of samples containing inorganic chlorides will be biased high due to partial recovery of inorganic species during combustion. Interference from inorganic species can be reduced by water washing the sample before analysis. This does not apply to water soluble samples.  
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1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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Standard Test Method for Water Using Volumetric Karl Fischer Titration

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4.1 Titration techniques using KF reagent are one of the most widely used for the determination of water.  
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Organic Compounds  
Acetals  
Ethers  
Acids (Note 1)  
Halides  
Acyl halides  
Hydrocarbons (saturated and unsaturated)  
Alcohols  
Ketones, stable (Note 4)  
Aldehydes, stable (Note 2)  
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Amides  
Orthoesters  
Amines, weak (Note 3)  
Peroxides (hydro, dialkyl)  
Anhydrides  
Sulfides  
Disulfides  
Thiocyanates  
Esters  
Thioesters  
Inorganic Compounds  
Acids (Note 5)  
Cupric oxide  
Acid oxides (Note 6)  
Desiccants  
Aluminum oxides  
Hydrazine sulfate  
Anhydrides  
Salts of organic and inorganic acids (Note 6)  
Barium dioxide  
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1.1 This test method is intended as a general guide for the application of the volumetric Karl Fischer (KF) titration for determining free water and water of hydration in most solid or liquid organic and inorganic compounds. This test method is designed for use with automatic titration systems capable of determining the KF titration end point potentiometrically; however, a manual titration method for determining the end point visually is included as Appendix X1. Samples that are gaseous at room temperature are not covered (see Appendix X4). This test method covers the use of both pyridine and pyridine-free KF reagents for determining water by the volumetric titration. Determination of water using KF coulometric titration is not discussed. By proper choice of the sample size, KF reagent concentration and apparatus, this test method is suitable for measurement of water over a wide concentration range, that is, parts per million to pure water.  
1.2 The values stated in SI units are to be regarded as standard.  
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1.4 Review the current Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid procedures, and safety precautions for chemicals used in this test procedure.  
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1.2 The Limit of Detection (LOD) is 0.18 units and the Limit of Quantitation (LOQ) is 0.59 units. Unit = hydroxyl number (OH#).
Note 2: LOD and LOQ were calculated using Standard deviations from 14.1.2.1.  
1.3 Review the current appropriate Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid procedures, and safety precautions.  
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4.1 Bisphenol A is used for production of polycarbonate or epoxy resin. The presence of impurities in bisphenol A is undesirable because they may slow down the polymerization and be impurities in the final product.  
4.2 Determination of the trace impurities, such as isomer of bisphenol A and the unreacted raw material, is often required. This test method is suitable for setting specifications and for using as an internal quality control where these products are produced or used.  
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4.2 Of the two test methods described, the pycnometer method (Test Method B, 1.1.2) is the most accurate and precise. For this reason it is the preferred method in case of disputes. The hydrometer method (Test Method A, 1.1.1) is the least accurate and precise, but it is also the simplest and fastest to perform and is often entirely satisfactory for many purposes. If the sample is too viscous to permit the hydrometer to float freely, the pycnometer test method should be used.
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1.1 These test methods cover the determination of the specific gravity, apparent, of liquid industrial chemicals. Two test methods are covered as follows:  
1.1.1 Test Method A, specific gravity, apparent, by means of a hydrometer.  
1.1.2 Test Method B, specific gravity, apparent, by means of a pycnometer.  
Note 1: Test Method D4052 describes an instrumental procedure.  
1.2 In common usage the term specific gravity, apparent, is understood to mean specific gravity.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in these test methods with the exception of Fahrenheit (°F) in 5.1 as an example of a possible industrial specification unit.  
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