ASTM D982-16(2022)
(Test Method)Standard Test Method for Organic Nitrogen in Paper and Paperboard
Standard Test Method for Organic Nitrogen in Paper and Paperboard
SIGNIFICANCE AND USE
4.1 The purpose of this test method is to determine the amount of organic nitrogen present within a sample of electrical insulation paper or paperboard. Nitrogen content is used to determine if the paper or paperboard has been chemically treated to withstand higher than normal operating temperatures. Such a paper or paperboard is referred to in the industry as “thermally upgraded.” A paper or paperboard that is thermally upgraded can withstand higher operating temperatures and allow the electrical equipment to have a longer useful life span.
SCOPE
1.1 This test method covers the determination of nitrogenous organic materials in paper and paperboard, which typically are used to reduce the thermal degradation of the cellulose in the paper and paperboard.
1.2 The nitrogen determination by this method does not include the nitrogen in nitro compounds, nitrates, nitrites, azo, hydrazine, cyanide, or pyridine ring-type compounds, none of which are normally found in paper and paperboard. There is no known modification of the method that is applicable to all nitrogenous compounds.
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 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.
General Information
Standards Content (Sample)
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.
Designation: D982 − 16 (Reapproved 2022) Technical Association of Pulp
and Paper Industry
Standard Method T 418 os-61
Standard Test Method for
Organic Nitrogen in Paper and Paperboard
This standard is issued under the fixed designation D982; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Summary of Test Method
1.1 This test method covers the determination of nitrog- 3.1 This test method is a modification of the well-known
Kjeldahl procedure. In this test method, compounds that yield
enous organic materials in paper and paperboard, which
typically are used to reduce the thermal degradation of the their nitrogen as ammonia are digested with concentrated
sulfuric acid, using sodium sulfate to raise the boiling point,
cellulose in the paper and paperboard.
and mercuric oxide as a catalyst. The organic matter is
1.2 The nitrogen determination by this method does not
destroyed and the nitrogen is fixed as ammonium sulfate in the
include the nitrogen in nitro compounds, nitrates, nitrites, azo,
excess acid.
hydrazine, cyanide, or pyridine ring-type compounds, none of
which are normally found in paper and paperboard.There is no
4. Significance and Use
known modification of the method that is applicable to all
4.1 The purpose of this test method is to determine the
nitrogenous compounds.
amount of organic nitrogen present within a sample of electri-
1.3 The values stated in SI units are to be regarded as
cal insulation paper or paperboard. Nitrogen content is used to
standard. No other units of measurement are included in this
determine if the paper or paperboard has been chemically
standard.
treated to withstand higher than normal operating tempera-
tures. Such a paper or paperboard is referred to in the industry
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard- as “thermally upgraded.” A paper or paperboard that is ther-
mally upgraded can withstand higher operating temperatures
ization established in the Decision on Principles for the
and allow the electrical equipment to have a longer useful life
Development of International Standards, Guides and Recom-
span.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
5. Apparatus
2. Referenced Documents
5.1 Kjeldahl Apparatus, with 500 mLor 800 mLflask and a
digestion rack, an efficient bulb or scrubber type of trap to
2.1 ASTM Standards:
ensure that no nonvolatile alkali is carried over, the trap being
D585 Practice for Sampling and Accepting a Single Lot of
connected to the flask with a rubber stopper and to the
Paper, Paperboard, Fiberboard, and Related Product
water-cooled condenser following, with rubber tubing. The
(Withdrawn 2010)
condenser tube shall be made of alkali-resistant glass or block
D644 Test Method for Moisture Content of Paper and
tin with the discharge end connected to a bent glass delivery
Paperboard by Oven Drying (Withdrawn 2010)
tube, the lower end of which is drawn out to a bore of about 3
mm.
This test method is under the jurisdiction of ASTM Committee D09 on 5.2 Other Apparatus—500 mL Erlenmeyer flask, 100 mL
Electrical and Electronic Insulating Materials and is the direct responsibility of
graduatedcylinder,50 mLburet,andmossyzincorglassbeads
Subcommittee D09.01 on Electrical Insulating Products.
for the flask to prevent bumping.
Current edition approved May 1, 2022. Published May 2022. Originally
approved in 1948. Last previous edition approved in 2016 as D982 – 16. DOI:
10.1520/D0982-16R22.
6. Reagents
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.1 Purity of Reagents—Reagent grade chemicals shall be
Standards volume information, refer to the standard’s Document Summary page on
used in all tests. Unless otherwise indicated, it is intended that
the ASTM website.
all reagents shall conform to the specifications of the Commit-
The last approved version of this historical standard is referenced on
www.astm.org. tee onAnalytical Reagents of theAmerican Chemical Society,
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D982 − 16 (2022)
where such specifications are available. Other grades are also heat the contents with a small flame or electric heater, taking
acceptable, provided it is first ascertained that the reagent is of care not to apply heat to the flask above the liquid level. An
sufficiently high purity to permit its use without lessening the asbestos-cement board with a hole cut to the proper diameter
accuracy of the determination. fortheflaskissuggested.Atfirstthemixturewillfrothandturn
black. Heat cautiously until frothing has ceased; then increase
6.2 Purity of Water—Unless otherwise indicated, references
the heat until the mixture boils gently. The black color
towatershallbeunderstoodtomeandistilledwaterorwaterof
gradually fades through brown to a colorless or almost color-
equal purity.
less solution. Continue heating for about 1 h after the solution
6.3 Boric Acid and Indicator Solution—Dissolve 43 g of
becomes colorless.
boric acid (H BO ) (free from borax), 6 mL of methyl red
3 3
NOTE3—Tominimizetheinevitableacidcondensationinthehoodwith
indicator, and 4 mL of methylene blue indicator, each 0.1 g in
this procedure, remove most of the acid fumes through a glass tube
100 mL of 95 % ethyl alcohol, per litre of freshly distilled
connected to a water aspirator.
water. Keep the solution in a borosilicate glass bottle. It is
9.2 Allow the solution to cool. It usually will solidify upon
stable for at least 6 months.
cooling to room temperature. When the solution starts to
NOTE 1—An alternative indicator mixture preferred by some for the
solidify or has cooled to room temperature, cautiously add
boric acid solution is 2 mLof methyl red and 10 mLof bromcresol green,
about 300 mL of water and 25 mL of the Na SO solution to
2 4
each 0.1 percent solution, in a 95 % ethanol (1) .
precipitate the mercury. Allow to stand 5 to 10 min with
6.4 Mercuric Oxide, HgO.
occasional shaking.
6.5 Sodium Hydroxide Solution (approximately 50 weight
NOTE 4—It has been reported that mercury sometimes volatilizes and
amalgamates with tin condenser tubes commonly used in the Kjeldahl
percent)—Dissolve 1030 g of sodium hydroxide (NaOH) in 1
apparatus. If the solution is allowed to stand a few minutes after the
L of water.
addition of the Na SO solution, volatilization of the mercury is likely to
2 4
6.6 Sodium Sulfate, anhydrous, powdered Na SO .
be negligible (2).
2 4
9.3 Add 50 mL of the boric acid and indicator solution to a
6.7 Sodium Thiosulfate Solution (80 g/litreL)—Dissolve 80
500 mL Erlenmeyer flask, connect the glass delivery tube to
g of sodium thiosulfate (Na S O ·5H O) in 1 L of water.
2 2 3 2
the discharge end of the condenser, and adjust th
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