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ASTM D6069-01

(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

Replaces
ASTM D6069-96 - Standard Test Method for Trace Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure Chemiluminescence Detection
Effective Date
10-Jun-2001
Replaced By
ASTM D6069-01(2006) - Standard Test Method for Trace Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure Chemiluminescence Detection (Withdrawn 2015)
Effective Date
01-Jun-2006

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ASTM D6069-01 - Standard Test Method for Trace Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure Chemiluminescence DetectionASTM D6069-01 - Standard Test Method for Trace Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure Chemiluminescence Detection
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ASTM D6069-01 - Standard Test Method for Trace Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure Chemiluminescence Detection
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D6069–01
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 * E 29 Practice for Using Significant Digits in Test Data to
4
Determine Conformance with Specifications
1.1 This test method covers the determination of total
E 691 Practice for Conducting an Interlaboratory Study to
nitrogen (organic and inorganic) in aromatic hydrocarbons,
4
Determine the Precision of a Test Method
their derivatives and related chemicals.
2.2 Other Documents:
1.2 This test method is applicable for samples containing
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
nitrogen from 0.2 to 2 mgN/kg. For higher nitrogen concen-
5
1910.1200
trations refer to Test Method D 4629.
1.2.1 The detector response of this technique within the
3. Terminology
specified scope of this test method is linear with nitrogen
3.1 Definitions:
concentration.
3.1.1 reduced pressure chemiluminescence—a chemical re-
1.3 The following applies to all specified limits in this test
action at pressure less than 760 mm mercury (Hg) in which
method: for purposes of determining conformance with this
light is emitted.
test method, an observed value or a calculated value shall be
3.1.2 oxidative pyrolysis—a process in which a sample
rounded off “to the nearest unit” in the last right-hand digit
under goes combustion in an oxygen rich environment at
used in expressing the specification limit, in accordance with
temperatures greater than of 650°C.
the rounding-off method of Practice E 29.
3.1.2.1 Discussion—Organic compounds pyrolytically de-
1.4 This standard does not purport to address all of the
compose to carbon dioxide, water and elemental oxides.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 A specimen is introduced into a gas stream, at a
bility of regulatory limitations prior to use. For specific hazard
controlled rate, and carried into a high temperature furnace
statements, see Section 9.
(>900°C) where an excess of oxygen is added. Pyrolysis
2. Referenced Documents converts organic material in the specimen to carbon dioxide
and water. Organic nitrogen and inorganic nitrogen com-
2.1 ASTM Standards:
pounds, present in the specimen, are converted to nitric oxide
D 1555 Test Method for Calculation of Volume and Weight
2 (NO). Nitric oxide reacts with ozone in the detector producing
of Industrial Aromatic Hydrocarbons
nitrogen dioxide molecules in an excited state. As the excited
D 3437 Practice for Sampling and Handling Liquid Cyclic
2 nitrogen dioxide molecules relax to ground state, light is
Products
emitted. This light is detected by a photomultiplier tube with
D 4629 Test Method for Organically Bound Trace Nitrogen
the resulting signal proportional to the concentration of nitro-
in Liquid Petroleum Hydrocarbons By Syringe/Inlet Oxi-
3
geninthesample.Operatingthedetectoratareducedpressure,
dative Combustion and Chemiluminescence Detection
lowers the probability of the excited nitrogen dioxide mol-
ecules colliding with other molecules before they undergo
chemiluminescence. Thus, reduced pressure provides im-
1
This test method is under the jurisdiction of ASTM Committee D16 on
proved sensitivity and lower noise.
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
Subcommittee D16.04 on Instrumental Analysis.
Current edition approved June 10, 2001. Published August 2001. Originally
4
published as D 6069 – 96. Last previous edition D 6069 – 96. Annual Book of ASTM Standards, Vol 14.02.
2 5
Annual Book of ASTM Standards, Vol 06.04. Available from the Superintendent of Documents, U.S. Government Printing
3
Annual Book of ASTM Standards, Vol 05.02. Office, Washington, DC 20402.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D6069
5. Significance and Use sample from vaporizing as it is injected into the boat. The
sample should start vaporizing as it enters the furnace. It is
5.1 This method has been prepared to detect and quantitate
critical that the sample vaporize at a constant and reproducible
nitrogen-containing compounds such as N-formylmorpholine
rate. Thi
...

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1.1 This test method covers the determination of organic chloride in aromatic hydrocarbons, their derivatives, and related chemicals.  
1.2 This test method is applicable to samples with chloride concentrations to 25 mg/kg. The limit of detection (LOD) is 0.2 mg/kg and the limit of quantitation (LOQ) is 0.7 mg/kg. With careful analytical technique or the measurement of replicates, or both, this method can be used to successfully analyze concentrations below the LOD.
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Standard Test Method for Water Using Volumetric Karl Fischer Titration

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4.4 Water can be determined directly in the presence of the following types of compounds:    
Organic Compounds  
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Ketones, stable (Note 4)  
Aldehydes, stable (Note 2)  
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Orthoesters  
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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  
Calcium carbonate  
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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.  
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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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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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1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 Consult current OSHA regulations, suppliers’ Safety Data Sheets, and local regulations for all materials used in this specification.  
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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.  
4.3 Purity is commonly reported by subtracting the determined expected impurities and water from 100 %. However, a HPLC analysis cannot determine absolute purity if unknown components are contained within the material being examined.
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1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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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.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Sections 8 and 16.  
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    7 pages
    English language
    sale 15% off
  • Standard
    7 pages
    English language
    sale 15% off