Astm D 202

An American National Standard
Designation: D 202 – 97 (2002)e1
Standard Test Methods for

Sampling and Testing Untreated Paper Used for Electrical
Insulation1
This standard is issued under the fixed designation D 202; 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.
This standard has been approved for use by agencies of the Department of Defense.
e1 NOTE—Editorial changes made to footnotes 13-15, and Section 1 September 2002.
1. Scope thetic, organic, or inorganic; and flexible polymeric binder

1.1 These test methods cover procedures for sampling and materials.
testing untreated paper to be used as an electrical insulator or 1.2 The procedures appear in the following sections:
as a constituent of a composite material used for electrical ASTM or TAPPI
Reference
insulating purposes. Procedure Sections (Modified)
1.1.1 Untreated papers are thin, fibrous sheets normally laid Absorption (Rise of Water) 78 to 83 ...
down from a water suspension of pulped fibers (usually Acidity-Alkalinity-pH 45 to 54 E 70
Air Resistance 98 to 101 D 726
cellulosic), which may contain various amounts of nonfibrous Aqueous Extract Conductivity 55 to 64 ...
ingredients, and which are calendared, if required, to obtain Ash Content 40 to 44 D 586
desired thickness and density. Nevertheless, these test methods Bursting Strength 102 to 107 D 774
Chlorides (Water-Extractable) 165 to 183 ...
are applicable, generally although not invariably, to papers Conditioning 15 D 6054
formed by other means, to papers modified (during or after Conducting Paths 138 to 151 ...
formation) by additions, and to papers given subsequent Density, Apparent 29 to 33 ...
Dielectric Strength 152 to 157 D 149
mechanical treatments such as creping. Dimensions of Sheet, Rolls and 16 to 24 D 374
1.1.2 As an electrical insulating and dielectric material, Cores
paper is considered “untreated” until it is subjected to a Dissipation Factor and Permittivity 158 to 164 D 150
Edge-Tearing Resistance 126 to 130 D 827
manufacturing process such as drying, impregnation, or var- Fiber Analysis 74 to 77 D 1030
nish treatment. Folding Endurance 108 to 110 T 423 and D2176
1.1.3 The test methods given herein were developed spe- Grammage 25 to 28 D 646
Permittivity 158 to 164 D 150
cifically for papers having a thickness of 0.75 mm (0.030 in.) Heat Stability in Air 131 to 137 D 827
or less. A number of these test methods are also suitable for use Impregnation Time 84 to 91 ...
on other materials such as pulps or boards. Refer to Test Internal-Tearing Resistance 121 to 125 D 689 or T414
Moisture Content 34 to 39 D 644 and D3277
Methods D 3376 or Methods D 3394 to determine which tests Particulate Copper 193 to 202 ...
are applicable to pulps or electrical insulating boards. In the Particulate Iron 184 to 192 ...
paper industry, some products in thicknesses of less than 0.75 Reagents 4 D 1193
Reports 14 E 29
mm are termed “paperboard”. Such products are included Sampling 6 to 13 D 3636
within the scope of these methods. Silver Tarnishing by Paper and 203 to 206 T 444
Paperboard
1.1.4 These test methods are applicable to flexible Solvent-Soluble Matter 65 to 73 ...
fibrous-mat materials formed from suspensions of fiber in Surface Friction 92 to 97 D 528 and T455
fluids other than water. These mats may have thicknesses Tensile Properties 111 to 120 D 76, E4
Thickness (see Dimensions) 16 to 24 D 374
approaching 2 mm, and may contain fibers that are natural,
synthetic, organic, or inorganic; fillers that are natural, syn- 1.3 The tests for Holes and Felt Hair Inclusions and the
Stain Test for Fine Pores, have been removed from this
compilation of test methods. These test methods were specific
1
These test methods are under the jurisdiction of ASTM Committee D09 on to grades of capacitor paper formerly covered by Specification
Electrical and Electronic Insulating Materials and are the direct responsibility of D 1930, which has been withdrawn.
Subcommittee D09.19 on Dielectric Sheet and Roll Products.
Current edition approved March 10, 1997. Published March 1998. Originally NOTE 1—This compilation of test methods is closely related to IEC
published as D 202 – 24 T. Last previous edition D 202 – 92. Publication 60554-2. Not all of the individual methods included herein are
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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Copyright ASTM International 1

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D 202 – 97 (2002)e1
included in IEC 60554-2, nor are all of the methods in IEC 60554-2 D 2753 Specification for Electrolytic Capacitor Paper3
included in this standard. The individual procedures as described in the D 2865 Practice for Calibration of Standards and Equip-
two standards are in general sufficiently close to each other that it is ment for Electrical Insulating Materials Testing7
reasonable to expect that test results obtained by most of the procedures
specified in either standard will not differ significantly. However, before
D 3277 Test Method for Moisture Content of Oil-
assuming that a procedure in these test methods is exactly equivalent to an Impregnated Cellulosic Insulation8
IEC 60554-2 procedure, the written procedures should be compared D 3376 Test Methods of Sampling and Testing Pulps to be
closely, and if it seems advisable, test results by the two procedures should Used in the Manufacture of Electrical Insulation7
be compared. D 3394 Test Methods for Sampling and Testing Electrical
1.4 This standard does not purport to address all of the Insulating Board7
safety concerns, if any, associated with its use. It is the D 3636 Practice for Sampling and Judging Quality of Solid
responsibility of the user of this standard to establish appro- Electrical Insulating Materials7
priate safety and health practices and determine the applica- D 6054 Practice for Conditioning Electrical Insulating Ma-
bility of regulatory limitations prior to use. See 43.2.1, 71.1, terials for Testing7
143.1, 148.1 and 156.1 for specific hazards. E 4 Practices for Force Verification of Testing Machines9
E 29 Practice for Using Significant Digits in Test Data to
2. Referenced Documents Determine Conformance with Specifications10
2.1 ASTM Standards: E 70 Test Method for pH of Aqueous Solutions with the
D 76 Specification for Tensile Testing Machines for Tex- Glass Electrode11
tiles2 2.2 TAPPI Standards:12
D 149 Test Method for Dielectric Breakdown Voltage and T 413 Ash in Paper and Paperboard
Dielectric Strength of Solid Electrical Insulating Materials T 414 Internal Tearing Resistance of Paper
at Commercial Power Frequencies3 T 423 Folding Endurance of Paper (Schopper Type Test)
D 150 Test Methods for AC Loss Characteristics and Per- T 444 Silver Tarnishing by Paper and Paperboard
mittivity (Dielectric Constant) of Solid Electrical Insulat- T 455 Identification of Wire Side of Paper
ing Materials3 T 470 Edge Tearing Resistance of Paper
D 374 Test Methods for Thickness of Solid Electrical Insu- 2.3 IEC Standard:
lation3 IEC 60554-2 Specification for cellulosic papers for electri-
D 528 Test Method for Machine Direction of Paper and cal purposes—Part 2: Methods of test13
Paperboard4
D 586 Test Method for Ash in Paper4 3. Terminology
D 644 Test Method for Moisture Content of Paper and 3.1 Definitions:
Paperboard by Oven Drying4 3.1.1 For definitions pertaining to sampling refer to Termi-
D 646 Test Method for Grammage of Paper and Paperboard nology D 1711 or to Practice D 3636.
(Weight Per Unit Area)4 3.1.2 For definitions pertaining to dissipation factor and
D 689 Test Method for Internal Tearing Resistance of Pa- permittivity refer to Terminology D 1711 or to Test Methods
per4 D 150.
D 726 Test Method for Resistance of Nonporous Paper to 3.2 Definitions of Terms Specific to This Standard:
Passage of Air4 3.2.1 air resistance, of paper, n—a paper property which
D 774 Test Method for Bursting Strength of Paper4 quantifies impediment to the transverse passage of air through
D 827 Test Method for Edge-Tearing Resistance of Paper5 the paper under specific conditions of test, and reported as
D 1030 Test Method for Fiber Analysis of Paper and Paper- either time for a specified volume per area of test or volume for
board4 a specified time per area of test.
D 1193 Specification for Reagent Water6 3.2.1.1 Discussion—It is expressed in terms of time (sec-
D 1389 Test Method for Proof-Voltage Testing of Thin onds) required for passage of a specified volume of air through
Solid Insulating Materials3 a known area of paper, or, as the volume of air passing through
D 1677 Methods for Sampling and Testing Untreated Mica the paper in a given length of time.
Paper Used for Electrical Insulation3 3.2.2 ash content of paper, n—the solid residue remaining
D 1711 Terminology Relating to Electrical Insulation3 after combustion of the paper under specified conditions,
D 2176 Test Method for Folding Endurance of Paper by the expressed as a percentage of the dry mass of the original
M.I.T. Tester4 specimen.
D 2413 Test Methods for Preparation and Electrical Testing
of Insulating Paper and Board Impregnated with a Liquid 7
Annual Book of ASTM Standards, Vol 10.02.
Dielectric3 8
9
10
2 11
Annual Book of ASTM Standards, Vol 07.01. Annual Book of ASTM Standards, Vol 15.05.
3 12
Annual Book of ASTM Standards, Vol 10.01. Available from the Technical Association of the Pulp and Paper Industry, 15
4
Annual Book of ASTM Standards, Vol 15.09. Technology Parkway, S., Norcross, GA 30092.
5 13
Discontinued 1981. See Annual Book of ASTM Standards, Vol 15.09. Available from Global Engineering Documents, 15 Inverness Way, East
6
Annual Book of ASTM Standards, Vol 11.01. Englewood, CO 80112-5704.
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D 202 – 97 (2002)e1
3.2.3 basis weight of paper—see grammage of paper. the result is expressed in degrees of angle of inclination of the
3.2.4 bursting strength of paper, n—the hydrostatic pressure plane which will cause the block to continue an initiated
required to produce rupture of a circular area of the material movement.
under specified test procedures. 3.2.14 tensile energy absorption of paper (TEA), n—the
3.2.5 coverage of paper, n—the reciprocal of grammage (or work performed when a paper specimen is stressed to break in
basis weight). tension under prescribed conditions, as measured by the
3.2.6 elongation of paper, n—the maximum tensile strain integral of the tensile stress over the range of tensile strain from
developed in the test specimen before break in a tension test zero to the strain corresponding to maximum stress, expressed
under prescribed conditions, calculated as the ratio of the as energy (work) per unit of original surface area of the test
increase in length of the test specimen to the original test span, specimen.
and expressed as a percentage. 3.2.14.1 Discussion—The TEA is expressed as energy
3.2.6.1 Discussion—It is calculated as the ratio of the (work) per unit of original surface area (length 3 width) of the
increase in length of the test specimen to the original test span, test specimen.
and is expressed as a percentage. 3.2.15 tensile strength of paper, n—the maximum tensile
3.2.7 folding endurance of paper, n—the resistance to stress developed in a test specimen in a tension test carried to
fatigue resulting from repeated folding under specified condi- break under prescribed conditions, expressed for thin papers as
tions of test, expressed as the number of double folds required force per unit original width of the test specimen.
to rupture a specimen, or as the logarithm of that number. 3.2.15.1 Discussion—Tensile stress is the force per unit of
3.2.7.1 Discussion—The level is expressed as the number of original cross-sectional area, but in thin materials such as paper
double folds required to rupture a specimen. Sometimes the it is commonly expressed in terms of force per unit of original
level is expressed as the logarithm of the number. width.
3.2.8 grammage of paper, n—the mass per unit area of 3.2.16 thickness of an electrical insulating material, n—the
paper, expressed as grams per square metre. perpendicular distance between the two surfaces of interest,
3.2.8.1 Discussion—Grammage is sometimes called weight determined in accordance with a standard method.
or basis weight of paper. These terms are most frequently used 3.2.16.1 Discussion—The thickness of papers under 0.05
when non-metric units are used, and the area is that of the mm (0.002 in.) in thickness, is often defined as one tenth that
paper in one of the several standard reams of papers defined of a stack of ten sheets in certain paper specifications.
within the paper industry. 3.2.17 water extract conductivity of paper, n—the apparent
volume conductivity at 60 Hz of a specimen of water that has
3.2.9 impregnation time of paper, n—the time in seconds
been used to dissolve water-soluble impurities from a specimen
required for a liquid of specified composition and viscosity to
of paper under prescribed conditions.
penetrate completely from one face of a sheet of paper to the
other under certain prescribed conditions. 4. Reagents
3.2.10 internal tearing resistance of paper, n—the force 4.1 Purity of Reagents—Use reagent grade chemicals in all
required to continue a previously-initiated tear across a speci- tests. Unless otherwise indicated, it is intended that all reagents
fied distance in a single thickness of paper, expressed as the conform to the specifications of the Committee on Analytical
average force per sheet to tear one or more sheets together. Reagents of the American Chemical Society, where such
3.2.10.1 Discussion—It is indicated on the specified appa- specifications are available.14 Other grades are acceptable,
ratus and reported as the average force per sheet to tear one or provided it is first ascertained that the reagent is of sufficiently
more sheets together across a specified distance. high purity to permit its use without lessening the accuracy of
3.2.11 loss on ignition of inorganic fiber paper, n—the the determination.
volatile and combustible fraction of a paper, expressed as a 4.2 Purity of Water—Except where otherwise indicated, use
percentage of the original dry mass lost upon ignition, using a reagent water, Type III, of Specification D 1193.
specified procedure.
5. Precision and Bias
3.2.11.1 Discussion—It is expressed as a percentage of the
original dry weight lost upon ignition, and is usually used 5.1 For individual test methods that follow, where no
instead of ash content when dealing with papers which are precision and bias section is included and where the procedure
principally composed of inorganic fibers. is contained in another standard to which reference is made,
3.2.12 solvent-soluble material in paper, n— the mass of refer to that standard for information relative to precision and
bias for that test method.
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material that can be extracted from a dry specimen by a

specified solvent under prescribed conditions, expressed as a SAMPLING
percentage of the original dry mass.
6. Scope
3.2.13 kinetic surface friction of paper, n— the ratio of the
force parallel to the surfaces of two pieces of paper in contact 6.1 This test method covers the procedure for judging lot
with each other to the force normal to the surfaces required to
continue previously-initiated movement relative to each other 14
“Reagent Chemicals, American Chemical Society PO Box 182426, Columbus,
at constant speed. OH 43218-2426.” For suggestions on the testing of reagents not listed by the
American Chemical Society, see “Reagent Chemicals and Standards,” by Joseph
3.2.13.1 Discussion—The test may be made using a paper- Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States
covered block on a paper-covered inclined plane, in which case Pharmacopeia.”

D 202 – 97 (2002)e1
TABLE 1 Number of Test Specimens per Test Unit; Number of Test Measurements per Test Specimen
Unit of Product—Roll, Pad, Unit of Product—Skid, Pallet, Box, Carton,
Bobbin, or Sheet Case, Package, Bundle, or Ream
Property Minimum Number Minimum Number

Number of Test Number of Test
of Test Measure- of Test Measure-
Specimens per Test Specimens per Test
ments per Test ments per Test
Unit Unit
Specimen Specimen
Aqueous extract conductivity, acidity-alkalinity-pH, ash, 2 1 2 1
moisture, solvent-soluble matter, chlorides, fiber analysis, surface
friction
Basis weight, bursting strength, folding endurance, tensile 10 1 10 1
properties, absorption
Thickness, dielectric strengthA 1 5 A
5 1
Holes and felt hair inclusions, dissipation factor, density, dry 1 1 1 1
coverage, core dimensions, sheet squareness
Conducting paths 5 1 5 1
Tearing strength 5 1 5 1
Air resistanceA 1A 10A 10 1
Impregnation time 6 1 6 1
Heat stability:
If folds or edge tear are used 10 1 10 1
If internal tear is used 5 1 5 1
Roll width, sheet dimensions 1 2 1 2
A
Indicates exception to number of specimens and test called for by the test method.
acceptability of electrical insulating papers. It is designed for 10.3 Inasmuch as several properties of paper (notably mois-
the purpose of determining acceptability of all or that portion ture content and aqueous extract conductivity) may change
of a shipment to a customer identified by a manufacturer’s lot with time, define a reasonable maximum time between receiv-
number. It is not intended to cover internal paper mill quality ing a lot of paper and testing it for such properties, either in the
control plans. This test method is intended for use in conjunc- material specification or by agreement between the seller and
tion with product specifications for electrical insulating papers. the purchaser.
10.4 For purposes of sampling for lot acceptance or rejec-
7. Summary of Test Method
tion, select the number of units of product from each lot in the
7.1 After Acceptable Quality Levels (AQLs) are agreed shipment in accordance with sampling plans selected from
upon for each of the various specification properties, sampling 10.2. Select units of product at random so as to be represen-
plans are selected and the basis for acceptance or rejection of tative of the lot. Take care to avoid selection of all units of
a lot of material is established. product from the top or bottom, one side or the other, or from
8. Significance and Use any specific location in the lot.
10.5 If more than one lot sample size is used, first determine
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8.1 In the buyer-seller relationship it is necessary that an those properties measured from the smaller sample, after which
understanding exists as to the expected nominal characteristics this sample may be included as part of the larger sample.
of the product, and the magnitude of permissible departure 10.6 Selecting Test Unit from Unit of Product:
from the nominal values. Also, it is necessary that an agree-
10.6.1 For units of product consisting of rolls 380 mm (15
ment be reached as to how many units of a lot can fall outside
in.) or more in width, take a test unit at least 0.5 m2 (5 ft2) in
of the specification limits without rejection of the lot. It is this
area, cut across the entire width of the roll.
latter subject that is addressed by this test method.
10.6.2 Cut test specimens from this area such that they
9. Establishing AQLs represent the entire width of the roll.
9.1 AQLs for each critical major and minor property are as 10.6.3 If the paper is available in rolls less than 380 mm in
mutually agreed upon between the manufacturer and the width, take a test unit at least 1.25 m (4 ft) in length and cut test
customer. If needed, establish group AQLs for given groups of specimens so as to be representative of the full width of the
properties; these too are mutually agreed upon between the roll.
manufacturer and the purchaser. 10.6.4 When the unit of product is defined as a sheet, take
the test unit from the sheet so that the entire width and length
10. Selection of Samples of the sheet are represented.
10.1 A number of paper properties are listed in Table 1, 10.6.5 Where the unit is defined as a skid, pallet, box,
together with the appropriate number of test specimens and test carton, case, package, bundle, or ream and contains paper in
measurements for each property. Use these values for guidance the following forms:
in determining sample sizes. 10.6.5.1 Sheet Form—Take the test unit in such a way that
10.2 From Table 2 select a sampling plan appropriate to the each test specimen is cut at random from the sheet and each
lot size and the agreed-upon AQL. Alternatively, refer to sheet is taken at random throughout the unit of product in order
Practice D 3636 for selection of a sampling plan. Refer to that the test unit is representative of the unit of product
Practice D 3636 for further information relative to the prin- (wherever applicable). Exclude the first 12 mm (1⁄2 in.) of paper
ciples and practices of sampling methods. from the top or bottom (or ends) from the sampling.

D 202 – 97 (2002)e1
TABLE 2 Sampling Plans of figures used in the material specification to express the
Lot Tolerance tolerances. (See the rounding Method of Practice E 29).
Lot Sample Acceptance Rejection Percent
Size Number Number Defective
(Pt)
CONDITIONING
AQL = 2.0 % (1.5 to 2.5)A 15. Conditioning
15 1 2 24
20 1 2 18
15.1 Condition samples in air at 50 6 2 % relative humidity
30 1 2 12.5 at a temperature of 23 6 2°C (73.4 6 3.6°F). Hold the samples
35 2 3 14.5 in the conditioned air for not less than 4 h prior to the tests, and
40 2 3 12.8
50 2 3 10.5
support them so as to allow a free circulation around each
sample. (See Practice D 6054).
AQL = 4.0 % (2.6 to 5.0)A
15.2 Make the following physical tests in the conditioned
7 1 2 45
10 1 2 34
atmosphere: thickness, basis weight, tensile strength, stretch
20 2 3 24 under tension, internal tearing resistance, bursting strength,
30 3 4 21 folding endurance, absorption, air resistance, impregnation
35 3 4 18
40 3 4 16
time, dimensions, surface friction, and edge-tearing resistance.
50 3 4 13 15.3 For work of such precision that the hysteresis in the
AQL = 8.0 % (5.1 to 10.0)A equilibrium moisture content may lead to appreciable error,
5 1 2 58
approach the moisture content equilibrium under standard
10 2 3 45 conditions from a drier state, following the preconditioning
15 2 3 32 provisions in Practice D 6054.
20 3 4 30
25 3 4 25
DIMENSIONS OF SHEETS, ROLLS, AND CORES
A
Refers to the range of AQL’s covered.
16. Scope
10.6.5.2 Roll, Pad, or Bobbin Form—Select the test unit at 16.1 These test methods cover procedures for the determi-
random from the rolls that make up the unit of product. (Do not nation of dimensions of sheets of electrical insulating paper;
include the first few turns of each roll as part of the test unit.) rolls of electrical insulating paper; and cores upon which rolls
of paper are wound.
11. Identification of Lot Sample Pieces 16.2 The length of any sheet is the dimension measured in
11.1 Mark each unit of product of the sample so that it can the machine direction of the paper, and the width of the sheet
be identified at any time. is the dimension measured in the cross-machine direction. The
thickness of any sheet is as defined in 3.1.18.
12. Lot Disposition
12.1 If the lot sample fails to meet the requirements for 17. Summary of Test Method
acceptability, the entire lot is subject to rejection. 17.1 Thickness measurements:
17.1.1 Three types of micrometers may be used for these
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13. Waiver of Requirements measurements; machinist’s micrometer with ratchet, dead-
13.1 The customer may agree to waive requirements with weight dial micrometer, or motor-operated micrometer.
respect to the sampling plans, conducting of tests, applicable 17.1.2 Measurements are made in prescribed manners, us-
property specified limits, or lot rejection. ing the micrometer designated for a particular case. The use of
a machinist’s micrometer is not recommended except for
REPORTS screening or rough measurements to be later confirmed by the
more accurate instruments designated herein.
14. Report 17.2 Sheet Length and Width, and Roll and Core
14.1 At the completion of testing, report the test results of Dimensions—Steel scales, vernier calipers, or go-no-go gages
the paper properties with identifying units on a report form that are used with conventional techniques to determine the width,
includes the following: length, and squareness of sheets, the width and diameter of
14.1.1 Identification of the paper sampled and tested by lot rolls, and the inside and outside diameters of cores.
number, type, grade, etc.,
14.1.2 Dates of testing, 18. Significance and Use
14.1.3 Location of the testing laboratory and the person 18.1 Accurate determination of thickness is important both
responsible for the testing, for acceptance tests and for design purpose. The number of
14.1.4 Remarks indicating test method or procedure used layers of paper required for a certain overall thickness of
and the deviation, if any, from the standard test procedures, and insulation depends on this dimension. Since apparent density is
14.1.5 Indication of the variance in test measurements such a function of weight per unit area and thickness, the latter must
as range, standard deviation, s, etc. be known in order to calculate apparent density. Thickness
14.2 Report the test results either as calculated or observed enters into the calculation of dielectric strength, resistivity, and
values rounded to the nearest unit in the last right-hand place other electrical properties.

D 202 – 97 (2002)e1
18.2 Essentially all paper is purchased with the other 21. Test Specimens
dimensions of the sheet or roll specified, with tolerances on 21.1 Take test specimens of sheets from the original
these dimensions. Compliance with these requirements is samples, conditioned flat in accordance with Section 15.
usually necessary for trouble-free use of the paper in manu- 21.2 For papers over 0.051 mm (0.002 in.) in nominal
facturing operations. thickness use a single sheet as a test specimen for thickness
18.3 The dimensions of rolls and of the roll cores determine measurements.
the weight that must be handled, and if the roll will physically 21.3 For papers 0.051 mm (0.002 in.) and under in nominal
fit on the payoff stand of the equipment on which it will be thickness, the specimen for thickness measurements may be a
further processed. single sheet or a stack of ten sheets as mutually agreed upon
19. Apparatus between the purchaser and the supplier.
19.1 Thickness: NOTE 3—In selecting the options given in 21.2 and 21.3, several factors
19.1.1 Determine the thickness using any one of the follow- are hereby given for consideration: (1) Greater reliability of micrometer
measurements is achieved when measurements are made on stack speci-
ing apparatus: mens. (2) The thickness of a ten-sheet stack of paper does not necessarily
19.1.1.1 Method A—Machinist’s Micrometer with ratchet bear a constant relationship to the thickness of a single sheet. (3)
or equivalent, as described in the Apparatus Section of Test Variations in a single-sheet thickness are largely hidden in stack measure-
Methods D 374. ments. (4) Differences between measurements are greater on single-sheet
19.1.1.2 Method C—Dead-Weight Dial Micrometer, as de- specimens than on stack specimens.
scribed in the Apparatus Section of Test Methods D 374. This 21.4 Use a single sheet as the test specimen for length,
apparatus is not to be used for papers under 0.05 mm (0.002 width, and squareness of sheets.
in.) in nominal thickness. 21.5 For paper in roll form, use the entire roll as a specimen.
19.1.1.3 Method D—Motor-Operated Micrometer, con- It is not necessary to condition this specimen prior to dimen-
forming to the following requirements. The apparatus shall be sion measurements.
a dead-weight(not spring-) actuated, dial-type, motor-operated
micrometer. It shall conform to the apparatus described in the 22. Procedure
Apparatus Section (Method B) of Test Methods D 374, except 22.1 Thickness:
that the capacity shall exceed 0.8 mm (0.03 in.). Design the 22.1.1 Requirements Applicable to all Methods:
motor-operating mechanism that controls the lowering of the 22.1.1.1 The procedure for using any micrometer requires
presser foot to ensure that the loading on the specimen created the presser foot and anvil surfaces be clean during measure-
by the falling presser foot is below the loading created by a ments, that proper calibration operations are performed, includ-
free-falling presser foot dropped from a height of 0.008 mm ing the construction of a calibration curve if necessary; and that
(0.0003 in.) above the specimen surface. dial-type micrometers be mounted on a solid level surface free
of excessive vibration.
NOTE 2—For example, any free-falling body dropped from a height of
0.008 mm will attain a maximum theoretical velocity of approximately 12 22.1.1.2 When the width of the sample permits, make all
mm/s (0.5 in./s). A presser foot dropping at a controlled velocity of 0.8 to measurements with edges of the presser foot and the anvil at
1.5 mm/s (0.03 to 0.06 in./s) will create a loading equivalent to the loading least 6 mm (0.25 in.) away from the edges of the specimen.
produced by a free-falling pressor foot dropped from heights of 0.000028 22.1.1.3 Take a specified number of measurements (mutu-
to 0.000119 mm (0.000001 to 0.000005 in.). ally agreed upon between the purchaser and the supplier) at
19.1.2 Calibrate micrometers in accordance with the Cali- regular intervals across the entire width of each specimen,
bration Section of Test Methods D 374. preferably in a line that is at right angles to the machine
19.2 Other Measurements: direction of the paper. In all cases make at least five such
19.2.1 Scale—A machinist’s precision steel scale of suitable measurements. Apply the deviations for the parts of the scale
length graduated to read within the accuracy specified for the corresponding to the paper thickness measured as corrections
sheet or roll size tolerances. A similar scale of suitable length to the thickness reading.
is also required to measure diagonals of sheets. 22.1.1.4 When using multiple-sheet test specimens, do not
19.2.2 Calipers—A machinist’s vernier caliper of suitable place the presser foot closer than 20 mm (0.75 in.) from any
size graduated to read within the degree of accuracy specified folded edge of the stack.
for the inside diameter tolerances of the core. 22.1.2 Method A—Determine the thickness in accordance
19.2.3 The measuring scales and calipers shall be graduated with the Procedure Section of Test Methods D 374.
so that half of the specified tolerance can be read directly, that 22.1.3 Method C:
is, if the tolerance is 1.0 mm (or 1⁄32in.) then the scale shall be 22.1.3.1 Place the specimen between the contact surfaces
graduated to at least 0.5 mm (or 1⁄64 in.) and lower the presser foot onto the specimen at a location
19.2.4 Gages—A set of two gages (“go” and “no-go”) for outside of the area to be measured. This will indicate the
each size core. Each gage in a set shall have a diameter within approximate thickness so that the conditions set forth herein
60.005 mm (0.0002 in.) of the specified maximum or mini- can be maintained.
mum diameter. 22.1.3.2 Raise the presser foot, move the specimen to the
measurement position, and lower the presser foot to 0.0075
20. Sampling mm (0.0003 in.) above the thickness obtained on the first
20.1 Sample in accordance with Sections 6 to 13. determination; then let the presser foot drop.
--`,,,`,`,`,`````,,,```,,`,,`,`-`-`,,`,,`,`,,`---

D 202 – 97 (2002)e1
22.1.3.3 For each succeeding measurement raise the presser 23.1.3 Squareness, reported as the difference in the lengths
foot, move the specimen to the next measurement location, and of the diagonals divided by the shorter length.
lower the presser foot to 0.0075 mm above the thickness 23.1.4 Roll Dimensions:
obtained on the first determination before letting the presser 23.1.4.1 Roll Width, reported as the average of the measure-
foot drop. ments for each specimen and,
22.1.3.4 An alternative technique is to lower the presser foot 23.1.4.2 Roll Diameter, reported as the average of the
at some velocity less than 13 mm/s (0.5 in./s) onto the surface measurements for each specimen.
of the paper specimen. 23.1.5 Core Dimensions:
22.1.3.5 When making thickness measurements, maintain 23.1.5.1 Number of cores that were within the limits of the
the presser foot dead weight loading on the test specimen for at go-no-go gages and the number that exceeded the limits of the
least 2 s, but not more than 4 s before taking the reading. go-no-go gages,
23.1.5.2 Measured inside diameters of cores not within the
NOTE 4—The procedure described in 22.1.3 minimizes small errors
present when the presser foot is lowered slowly onto the specimen. limits for inside diameter (if specified) and,
NOTE 5—When measuring the thickness of noticeably compressible 23.1.5.3 Average outside diameter of cores (if specified).
papers, the purchaser and the supplier may wish to fix the exact time,
within the above limits, that the pressure is applied to the test specimen. 24. Precision and Bias
22.1.4 Method D—Using the motor-operated micrometer, 24.1 Precision—This test method has been in use for many
follow the procedures described in 22.1.3. Place the specimens years, but no statement for precision has been made, and no
between the presser foot and the anvil and obtain thickness activity is planned to develop such a statement.
readings. When making thickness measurements, maintain the 24.2 Bias—A statement of bias cannot be made because of
deadweight loading on the test specimen for at least 2 s but not the lack of a standard reference material.
more than 4 s before taking a reading. GRAMMAGE (WEIGHT PER UNIT AREA) AND DRY
COVERAGE
--`,,,`,`,`,`````,,,```,,`,,`,`-`-`,,`,,`,`,,`---
NOTE 6—When measuring the thickness of noticeably compressible

papers, the purchaser and the supplier may wish to fix the exact time,
within the above limits, that the proper pressure is applied to the test 25. Scope
specimen as well as the exact velocity of the fall of the presser foot. 25.1 This test method covers the determination of the
22.2 Length and Width of Sheets—Measure the length and weight (or mass) per unit area of paper.
width of the specimen to the nearest appropriate unit. Make 25.2 The weight per unit area is reported in any of several
two measurements in each dimension. units, such as grams per square metre, pounds per square foot
22.3 Squareness of Sheets—Measure the lengths of both (or per 1000 square feet), or pounds per ream. For most paper
diagonals of the sheet. products these are the more customary units. Test Method
22.4 Roll Dimensions: D 646 provides conversion factors for calculating results in
22.4.1 Measure the width of the specimen to the nearest these units.
appropriate unit. Make at least two measurements.
22.4.2 Measure the outside diameter of the specimen at least
two points on each end of the roll. 26.1 The area of several sheets of paper is determined from
22.5 Core Dimensions: linear measurements and the mass (commonly called “weight”)
22.5.1 Measure the inside core diameter at each end with is determined by weighing. The grammage is calculated from
go-no-go gages to determine whether the core meets the the ratio of the mass to the area.
minimum and maximum specified diameters. Measure cores 27. Significance and Use
having diameters outside of the specified limits at least two
points on each end with an inside feeler gage or the vernier 27.1 Knowledge of the grammage is useful in the selection
calipers. of materials for economical design purposes, product specifi-
22.5.2 Measure the outside core diameter at least two points cation, and routine area calculations.
on each end with the vernier calipers. 28. Procedure
23. Calculation and Report 28.1 Grammage—Determine the grammage in accordance
23.1 Report in accordance with Section 14, and include the with Test Method D 646, except sample the material in
following information, as applicable: accordance with Sections 6 to 13 of these test methods. Report
23.1.1 Thickness: the results in grams per square metre, or as otherwise specified.
23.1.1.1 Report the average, the minimum, and the maxi- 28.2 Dry Coverage—Proceed as in 28.1, cutting the speci-
mum of the individual readings for single-sheet specimens. men to the prescribed dimensions after conditioning in accor-
23.1.1.2 For multiple-sheet test specimens, divide the mi- dance with Section 15, and then drying the specimens to
crometer readings by the number of sheets in the specimen constant weight using the techniques described in Test Method
stack and use the resulting quotient as the individual “single D 644. Calculate the coverage as square metres per gram of
sheet” thickness. In all cases where multiple-sheet stacks are oven-dry weight.
used report the number of sheets in the stack. NOTE 7—Commercially, coverage is expressed as square inches per
23.1.2 Sheet Size, reported as the average of the measure- pound of oven-dry weight. Multiply square metres per gram of oven-dry
ments in each dimension. weight by 703 3 10 3 to convert to commercially used units.

D 202 – 97 (2002)e1
APPARENT DENSITY 35. Summary of Test Method
35.1 Oven-Drying Procedure—Specimens of paper are
29. Scope
weighed initially and after oven drying to equilibrium weight.
29.1 This test method covers procedures for measuring and The moisture content is calculated as a percentage of the initial
calculating the apparent density of paper. Two test methods for weight.
calculating and reporting the density are described. 35.2 Solvent-Extraction Procedure—Water is extracted
29.2 See also the procedures given in Section 163, relating from the specimen using an organic solvent. The water content
density to dissipation factor and permittivity. of the solvent is then determined using the Karl Fischer
titration procedure.
30.1 The volume and the weight of the test specimen are 36. Significance and Use
determined and used to calculate the density of the specimen in 36.1 A knowledge of moisture content is necessary to
grams per cubic centimetre. Either the conditioned weight or calculate, to a dry basis, analytical results obtained from
the oven-dried weight of the specimen is used, as specified. conditioned specimens. The moisture content affects cost when
purchasing papers, and is important in the design of electrical
31. Significance and Use insulating systems, since it affects properties such as shrinkage
31.1 The apparent density of untreated paper used for characteristics. Moisture content has a significant effect on
electrical insulating purposes describes the weight-to-volume many of the physical, electrical, and thermal aging properties
ratio of the paper, the weight and volume being determined of insulating papers, including runability on processing equip-
according to certain prescribed conditions. A knowledge of this ment.
property is useful in the design of electrical insulating systems 36.2 For applications involving paper in manufacturing,
and in determining the economic aspects of paper use. Many fabricating, and converting operations, use the oven-drying
physical and electrical properties of paper are related to procedure (Procedure A). This includes virtually all specifica-
apparent density. tion and quality control, and many research situations.
36.3 For paper impregnated with insulating fluid, or sub-
32. Procedure jected to a drying operation, the solvent-extraction procedure
32.1 Procedure A, Wet-Wet Density—Prepare three rectan- (Procedure B) may be applicable. In most cases this will be in
--`,,,`,`,`,`````,,,```,,`,,`,`-`-`,,`,,`,`,,`---
gular test specimens, of such size that the width and length can research or trouble-shooting applications.
be measured to within 6 1 %. Condition the specimens in
accordance with Section 15. Measure the thickness, length, and 37. Sampling and Preparation of Test Specimens
width in accordance with Sections 16 to 24. Determine the 37.1 Sample in accordance with Sections 6 to 13 of these
weight and calculate the density. The average density of the test methods.
three specimens is the test result. 37.2 Use procedures for sampling and specimen preparation
such that exposure of the test material to the open air, and
NOTE 8—If the dimensions are measured in inches, multiply the
calculated volume in cubic inches by 16.387 to obtain cubic centimetres.
resultant changes in moisture content, are minimized.
37.3 Prepare test specimens as specified in Test Method
32.2 Procedure B, Wet-Dry Density—The technique for D 644 or Test Method D 3277, as applicable.
obtaining wet-dry apparent density is identical with that
described in 32.1, except obtain the weight of the specimens 38. Procedures
after drying to a constant weight in an oven at 105 6 3°C as in 38.1 Procedure A—Determine the moisture content in ac-
Test Method D 644. cordance with Test Method D 644.
38.2 Procedure B—Determine the moisture content in ac-
cordance with Method D 3277, using Method A or Method B
33.1 Precision—The precision of this test method has not of that method, as applicable.
been determined. However, it is dependent upon the precision
with which the four separate measurements entering into the 39. Report
calculations are made, and upon the atmospheric conditions, 39.1 Report the moisture content as a percentage of the
particularly the relative humidity, in which the specimens are initial weight of the specimen, or, in the case of oil-
conditioned prior to test. impregnated materials, in accordance with Test Method
33.2 Bias—A statement of bias is not practicable because of D 3277.
lack of a standard reference material. 39.2 Report in accordance with Section 14, and the report
section of Test Method D 644 or Test Method D 3277, as
MOISTURE CONTENT applicable.
34. Scope ASH CONTENT
34.1 This test method covers two procedures for determin-
ing the mass percent of moisture in paper. The oven-drying 40. Scope
procedure is used for most applications, and the solvent- 40.1 This test method covers two procedures: Procedure A
extraction procedure is for oil-impregnated samples. for the determination of the noncombustible portion of paper,

D 202 – 97 (2002)e1
usually applied to cellulosic papers which have a small amount 44.3 Procedure B has no bias because the loss on ignition is
of residue after combustion; and Procedure B for the determi- defined in terms of this test method.
nation of loss on ignition of papers having high percentages of
inorganic material and which do not entirely lose their physical
integrity during ignition.
41. Summary of Test Methods
41.1 Procedure A—The weighed, oven-dried specimen is
ignited at a constant temperature in a covered crucible to
constant weight. The weight of the noncombustible residue is
determined and expressed as a percentage of the original
oven-dried weight.
41.2 Procedure B—A gas burner is used to burn off volatile
matter from an oven-dried specimen held in the burner flame.
The weight loss during this procedure is determined and
expressed as a percentage of the original weight.
--`,,,`,`,`,`````,,,```,,`,,`,`-`-`,,`,,`,`,,`---
42. Significance and Use

42.1 The ash determination is a relatively simple and
FIG. 1 Stirrer
convenient method to detect the presence of inorganic fillers,
coatings, pigments, or contaminants in paper. This test method
is also useful to prepare specimens for the quantitative deter- ACIDITY-ALKALINITY-pH
mination of inorganic constituents in paper. This procedure is
45. Scope
suitable for control testing, research, and referee analysis. The
specified ashing temperature is selected to minimize loss of 45.1 This test method is designed to indicate the active and
those inorganic constituents that are volatile at higher ashing the total acidity or alkalinity of an aqueous extract of electrical
temperatures. insulating papers. Since the aqueous extracts of most untreated
42.2 The loss-on-ignition procedure is useful as a quality papers used for electrical insulation are normally unbuffered
control test for papers having high levels of inorganic materials and are readily affected by atmospheric conditions, this method
in their structures. Do not use for papers having volatile or embodies features to minimize error from this source.
combustible contents greater than 75 %. 46. Summary of Test Method
43. Procedure 46.1 This test method consists of a hot-water extraction of
43.1 Procedure A—Determine the ash content in accor- the specimen followed by a pH measurement or an alkalinity-
dance with Test Method D 586, except use 575 6 25°C as the acidity titration of the extract solution.
ashing temperature.
43.2 Procedure B: 47. Significance and Use
43.2.1 Precaution—Perform this test in an exhausted fume 47.1 The pH determination measures the extent to which the
hood. Avoid inhaling any of the products of combustion. paper alters the hydrogen-hydroxyl ionic equilibrium of pure
43.2.2 Cut a specimen approximately 100 by 150 mm (4 by water. The acidity-alkalinity determination measures the quan-
6 in.). Oven dry the specimen to constant weight at 100 6 5°C. tity of extracted ionic material that contributes to that equilib-
Record the oven dry weight (Wod) to the nearest milligram. rium change. Such constituents may represent potential short-
43.2.3 Burn off the volatile matter over a Meker-type burner comings, either initially, or after prolonged service, of
in such a manner as to avoid melting the inorganic fibers and electrical equipment using this paper. These tests are useful for
thus entrapping volatiles. A properly ignited residue appears routine acceptance testing, research work or in the evaluation
white with no trace of carbon residue. of different materials.15
43.2.4 After burning off the volatiles, cool the specimen and
immediately weigh it to the nearest milligram. This is the ash 48. Apparatus
weight (Wa). 48.1 Bath—A hot-water bath.
43.2.5 Calculate the percent loss on ignition: 48.2 Motor and Stirrer—A motor with a stirrer constructed
as shown in Fig. 1. Use an acid- and alkali-resistant stirrer.
% loss on ignition 5 ~Wod 2 Wa!/Wod 3 100 (1)
Chromium-plated brass is a suitable material.
43.2.6 Report the loss on ignition to the nearest 0.1 %, in 48.3 Thermometers—Thermometers having a range from
accordance with Section 14. 50 to 100°C and graduated in 1° intervals.
44. Precision and Bias 48.4 Buret—A 10-mL buret graduated to 0.05 mL.
48.5 Electric Hot Plate.
44.1 For the precision and bias of Procedure A, refer to Test
Method D 586.
44.2 The precision of Procedure B has not been determined, 15
See Paper and Paperboard—Characteristics, Nomenclature, and Significance
and no activity is planned to determine its precision. of Tests, ASTM STP 60-B, ASTM, 1963, pp. 59–61.

D 202 – 97 (2002)e1
48.6 Suction Filtering Apparatus. where:
48.7 pH Meter—A pH meter conforming to the require- E = NaOH equivalent (in millilitres) to 1 mL of H2SO4,
ments prescribed in Test Method E 70. A = NaOH solution required (corrected), mL, and
B = H2SO4 taken, mL.
49. Reagents
50. Test Specimen
49.1 Purity of Water—Use water in this test method that
meets the requirements described in 4.2, and is free of carbon 50.1 From the sample obtained in accordance with Sections
dioxide, and with a pH between 6.2 and 7.2 at 25°C. 6 to 13, cut a composite test specimen, weighing at least 5 g,
49.2 Buffer Solution, Standard (for standardizing the glass into small pieces approximately 0.4 in. (10 mm) square.
electrode)—Dry about 6 g of potassium acid phthalate for not Thoroughly mix the specimen. During preparation, avoid any
less than 2 h at 120°C. Cool in a desiccator. Add 5.0905 g of contamination by handling.
the salt to 500 mL of water at 25°C. The pH of this buffer
solution is 4.0 at 25°C. 51. Procedure
49.3 Indicator Solution—Add approximately 500 mg of 51.1 Place a 1-g portion of the composite specimen in a
neutral red to 300 mL of denatured ethanol. When it is 250-mL wide-mouth Erlenmeyer flask and add 100 mL of
thoroughly dissolved, dilute with ethanol to 500 mL in a boiling water. Clamp the flask in position in a boiling water
volumetric flask. Stopper the flask and allow to age overnight bath so that at least one half of the flask is immersed in the
at room temperature. Filter the aged liquid through a fritted water bath. During the stirring, maintain the temperature of the
glass filter using suction if necessary. Measure the pH of this contents of the flask at 95°C or above. Mount the stirrer so that
solution and, if necessary, adjust to pH 7.0 by the addition of the blades are within 10 mm (0.4 in.) of the bottom of the flask.
0.10 N NaOH solution. The assembled extraction apparatus is shown in Fig. 2. Drive
49.4 Sodium Hydroxide, Standard Solution (0.005 N)— the stirrer at a speed of 4000 to 5000 r/min for 5 min. At the
Dissolve 0.2 g of sodium hydroxide (NaOH) in water and end of this period the specimen should have been thoroughly
dilute to 1 L in a volumetric flask. To standardize, prepare 250 pulped. For papers unusually difficult to pulp increase the
mL of a 0.005 N potassium acid phthalate solution by period of stirring to 10 min.
dissolving 0.2552 g of the dried salt in water and making up to 51.2 Immediately after the specimen has been pulped, filter
the mark in a 250-mL volumetric flask at 20°C. (Do not dry the the contents of the flask rapidly with vacuum through a
salt at a temperature above 125°C). Pipet 25 mL of this solution perforated porcelain disk, refiltering the first portion of the
into a 250-mL flask. Add 25 mL of water. Immerse the pH filtrate to permit the formation of a mat. Do not wash the
electrode or if an indicator is used, add a few drops of indicator residual pulp.
solution. Pass nitrogen through the solution for 10 min. Titrate NOTE 10—It is important to accomplish filtration of the extract as
in a closed system with the standard NaOH solution to pH 7 or promptly as possible after the disintegration. When the fibers are too short
to an orange shade. If preferred, the potassium acid phthalate to form a satisfactory mat on the perforated porcelain disk, filter with
solution may be heated to boiling and titrated immediately, suction through a fine quantitative filter paper that has been washed twice
taking care that the temperature does not fall below 80°C in a Buchner funnel with 100-mL portions of boiled water.
during the titration. Run three specimens in the above way at 51.3 Immerse the electrode assembly in the hot (95 to
each standardization of the NaOH solution. Determine a blank 100°C) extract solution and determine the pH. For acidity or
on the same volume of water and indicator and deduct from the alkalinity determinations add the standardized (see 49.4 and
titration obtained above. Calculate the normality of the NaOH 49.5) alkali or acid, depending on the level of the pH
solution as follows: measurement. Carry out the acidity or alkalinity titration to an
Normality of NaOH solution 5 ~25 end point of pH 7.0 as indicated by the pH meter. If a
3 0.005!/mL 1 NaOH solution required colorimetric indicator is used for end point determination, add
(2) a few drops to the extract solution. The color will determine
NOTE 9—Good laboratory practice requires use of a freshly prepared
whether or not the extract is acid or alkaline.
and standardized NaOH solution. 51.4 Neutral red is a deep yellow under alkaline conditions
and deep red under acid conditions. Take the end point when
49.5 Sulfuric Acid, Standard (0.005 N)—Prepare 0.005 N the solution is orange. Experience indicates that pH at this
sulfuric acid (H2SO4) and determine the alkali equivalent of point is 6.8 to 7.2.
the acid as follows: Transfer 10 mL of the acid to a 250-mL
Erlenmeyer flask and dilute with 100 mL of water. Titrate in a NOTE 11—For routine control work, 0.01 N H2SO 4 may be used for
closed system or at the boiling point with the standard NaOH titrations.
solution as described in 49.4 for the standardization of the 51.5 Blank—Make a blank determination in parallel with
NaOH solution. Determine a blank on the same volume of the actual determination, using a volume of water equal to that
water and indicator solution and deduct from the titration of the extract at the end point, and subjecting it to the same
obtained above. Calculate the NaOH equivalent of the acid as conditions of temperature, agitation, etc., as the extract. Use
follows: the values for the blank measurement in the calculations in
E 5 A/B (3) 52.1.
--`,,,`,`,`,`````,,,```,,`,,`,`-`-`,,`,,`,`,,`---

D 202 – 97 (2002)e1
--`,,,`,`,`,`````,,,```,,`,,`,`-`-`,,`,,`,`,,`---
FIG. 2 Assembled Extraction Apparatus
52. Calculation W = mass of paper specimen, g.

52.1 Four combinations of conditions that affect the calcu- 52.2 Determine the acidity or alkalinity of the extract and
lations can exist. These are included in 52.1.1 through 52.1.4, the blank from the reading of the pH meter, or the color of the
with the appropriate calculation procedure combining extract indicator, before the titration is made, as indicated in 51.4.
and blank titration values for each: 52.3 It is assumed that the volume required for the titration
52.1.1 Acid Extract and Acid Blank: of the blank will be less than that required for the titration of
M 5 @~a 2 b! 3 N#/W (4) the extract. Under this assumption the calculated values for M
in 52.1.1 and 52.1.2 are in milliequivalents of acid, and the
52.1.2 Acid Extract and Alkaline Blank: values for M in 52.1.3 and 52.1.4 are in milliequivalents of
M 5 @~a 1 ~d 3 E!! 3 N#/W (5) alkali per gram of paper.
52.1.3 Alkaline Extract and Acid Blank: 53. Report
M 5 @~~c 3 E! 1 b! 3 N#/W (6) 53.1 Report in accordance with Section 14.
52.1.4 Alkaline Extract and Alkaline Blank: 54. Precision and Bias
M 5 @~c 2 d! 3 E 3 N#/W (7) 54.1 Precision—This test method has been in use for many
where: years, but no statement for precision has been made, and no
M = milliequivalents of acid or alkali per gram of speci- activity is planned to develop such a statement.
men, 54.2 Bias—This procedure has no bias because the values
N = normality of standard NaOH solution for acidity, alkalinity, and pH are defined in terms of this test
E = NaOH equivalent to 1 mL of H2SO4(see 49.5), mL, method.
a = NaOH solution to titrate an acid extract, mL,
AQUEOUS EXTRACT CONDUCTIVITY
b = NaOH solution to titrate an acid blank, mL,
c = H2SO4 to titrate an alkaline extract, mL, 55. Scope
d = H2SO4 to titrate an alkaline blank, mL,
55.1 This test method determines the electrical conductivity

D 202 – 97 (2002)e1
imparted to reagent water by boiling a specimen of paper in the mounted and adequately protected so that their relative posi-
water under carefully defined conditions. tions will not be affected by handling or moderate jarring. The
area of each electrode is to exceed 20 mm2. Construct the cell
so that the electrodes will be completely immersed on dipping
56.1 A specimen of paper is boiled while being agitated in the cell into the liquid medium. Platinize the electrodes (see
reagent water and the electrical conductivity of the water is 61.2) to make measurements at low frequency (60 Hz). At a
then determined. A blank determination is also made and the frequency of 1 kHz this precaution is unnecessary.
appropriate correction made to obtain the reported result.
59. Reagents
59.1 Reagent Water—In preparing the extract and KCl
57.1 The conductivity of the water extract of insulating solutions, use deionized water having a conductivity not
paper results from electrolytic impurities in the paper which greater than 1.0 µS/cm at 25 6 0.5°C when boiled and tested
may be present as ionizable acids, bases, salts, or a combina- in accordance with the procedure described in Section 62 in the
tion of these. These impurities are residues from the manufac- absence of a paper sample. Alternatively, prepare reagent water
turing process which have been incompletely removed. The by double distillation, the second distillation being over alka-
presence of excessive amounts of electrolytic impurities is line permanganate. Use acid- and alkali-resistant glass appara-
undesirable, as they tend to lower insulation resistance and tus for those distillations.
have corrosion-producing tendencies under conditions of ap- 59.2 Potassium Chloride Solution (0.01 M)—Prepare a
plied electrical potential. The fact that the conductivity of 0.01 M solution with reagent grade potassium chloride (KCl)
high-purity kraft papers may increase after manufacture, for as which has been dried for 2 h at 110°C. After cooling, dissolve
yet undetermined reasons, should be recognized in all com- 0.7455 g of the dried salt in reagent water and make up to 1 L
parisons of data. This test method is suitable for routine in a volumetric flask at 20°C.
acceptance tests, control tests, and research tests.
60. Test Specimen
58. Apparatus
60.1 From the samples obtained in accordance with Sec-
58.1 Conductivity Bridge—A 60-Hz ac conductivity bridge tions 6 to 13, cut a composite test specimen, weighing at least
or resistance indicator capable of measuring resistances up to 1 5 g into small pieces approximately 0.4 in. (10 mm) square.
MV with an accuracy of 65 %. Bridges operating at other Thoroughly mix the specimen, and during preparation avoid
frequencies, with equivalent accuracy may be used where any contamination by handling.
specified.
61. Preparation and Calibration of Conductivity Cell
NOTE 12—A convenient way to check the accuracy of the bridge is with
precision resistors of 61 % accuracy.
61.1 If unplatinized, clean a new cell with warm chromic
acid solution, wash thoroughly with reagent water, and rinse
58.2 Motor and Stirrer—A motor with a stirrer constructed with alcohol and ether. If the electrodes are already platinized,
as shown in Fig. 1. Use an acid- and alkali-resistant stirrer. omit the chromic acid wash.
Chromium-plated brass is a suitable material. 61.2 To platinize the electrodes, immerse the cell in a
58.3 Constant-Temperature Bath—A water bath maintained solution of 3.0 g of chloroplatinic acid and 0.010 g of lead
at 25 6 0.5°C. acetate in 100 mL of reagent water. Electrolyze, using a current
58.4 Beakers—Acid- and alkali-resistant glass 125-mL tall- density of 30 mA/cm 2, for 8 min, reversing the current every
form beakers, or any beakers of such dimensions that when the 2 min. Wash the electrodes thoroughly with reagent water (see
dip cell is immersed in 100 mL of liquid contained therein, the 59.1). To test for completeness of removal of electrolyte,
electrodes are fully covered. immerse the cell in 50 mL of reagent water and measure the
58.5 Flasks—Acid- and alkali-resistant glass, wide-mouth, resistance initially and at the end of 10 min. If a decrease in
250-mL Erlenmeyer flasks. resistance occurs, repeat the washing. Keep the cell immersed
58.6 Suction Filtering Apparatus. in reagent water when not in use.
58.7 Perforated Disk—A perforated porcelain or fritted 61.3 To determine the cell constant, place a beaker contain-
glass disk 50 mm in diameter with its edge beveled at an angle ing 0.01 M KCl solution (see 59.2) in the constant-temperature
--`,,,`,`,`,`````,,,```,,`,,`,`-`-`,,`,,`,`,,`---
of 60°, and having approximately 90 perforations, each ap- bath maintained at 25 6 0.5°C. After thermal equilibrium is
proximately 1 mm in diameter. established, measure the resistance of this solution. Calculate
58.8 Funnel—An acid- and alkali-resistant glass funnel the cell constant, K as follows:
having a top diameter of 100 mm and made with an exact 60°
angle. K 5 C 3 R cm21 (8)
58.9 Thermometers—One thermometer having a range where:
from − 10 to + 110°C and graduated in 1°C intervals (for R = resistance measured, V, and
extract solution), and one thermometer having a range from − 5 C = conductivity of the potassium chloride solution. The
to + 50°C and graduated in 0.1°C intervals (for constant- value for C, at 25°C is 1.41 3 10−3 S/cm.
temperature bath).
58.10 Electric Hot Plate. 62. Procedure
58.11 Conductivity Cell—Use a dip-type cell with a cell 62.1 Place a 1-g portion of the composite specimen in the
constant of 0.1 cm−1 with platinum electrodes securely 250-mL Erlenmeyer flask and add 100 mL of boiling reagent

D 202 – 97 (2002)e1
water. Clamp the flask in position in a boiling-water bath so 64. Precision and Bias
that at least one half of the flask is immersed in the water-bath. 64.1 This test method has been in use for many years, but no
During the stirring, maintain the temperature of the contents of statement for precision has been made and no activity is
the flask at 95°C or above. Mount the stirrer so that the blades planned to develop such a statement.
are within 10 mm (0.4 in.) of the bottom of the flask. The 64.2 This procedure has no bias because the value for
assembled extraction apparatus is shown in Fig. 2. Drive the aqueous extract conductivity is defined in terms of this method.
stirrer at a speed of 4000 to 5000 r/min for 5 min. At the end
of this period the specimen should have been thoroughly SOLVENT-SOLUBLE MATTER
pulped. For paper unusually difficult to pulp, increase the 65. Scope
period of stirring to 10 min.
65.1 This test method covers a procedure for determining
62.2 Immediately after pulping the specimen, filter the the weight percentage of material removable from a specimen
contents of the flask rapidly with suction through the 50-mm of paper, using a solvent-extraction method.
perforated porcelain disk supported in the 100-mm glass
funnel. Refilter the first portion of the filtrate after a satisfac- 66. Summary of Test Method
tory mat has formed on the disk. Do not wash the residual pulp. 66.1 A Soxhlet extraction apparatus is used, with appropri-
NOTE 13—If the fibers are too short, it may be impossible to form a mat ate volatile solvent to extract soluble material from the
on the bare porcelain disk. In this event place a 55-mm quantitative filter specimen. After extraction, the solvent is evaporated, and the
paper on the disk. Before using, wash the filter paper twice with 100-mL nonvolatile residue is weighed and calculated as a percentage
portions of hot reagent water. A Gooch-type crucible with a fritted-glass of the original weight of the specimen.
disk may also be used if the fibers are too short.
NOTE 14—It is important to accomplish filtration of the extract as 67. Significance and Use
promptly as possible after disintegration. 67.1 Solvent-extractable materials in electrical insulating
62.3 After the filtration, dilute the extract solution to 100 paper include various contaminants which may be present in
mL with hot reagent water by bringing it up to the mark in a the raw material. If present in sufficient quantity, these mate-
100-mL graduated cylinder. Transfer to the tall-form beaker to rials may lower the quality of the insulation or have deleterious
make the conductance measurement. Stopper the beaker with effects on the electrical characteristics of the liquid compounds
an aluminum foil- or tin foil-covered rubber stopper and place used in contact with the paper in various types of electrical
in the water bath maintained at 25 6 0.5°C. apparatus. Ethanol-soluble materials in capacitor paper are
found to increase the electrical conductivity of some dielectric
62.4 As soon as thermal equilibrium is established, place
fluids which are used as impregnants in capacitors.
the dip cell in the extract solution, making certain that the
67.2 This test method, with a specified solvent, may be used
electrodes are completely immersed. Measure the resistance on
for routine acceptance and for research tests.
the most sensitive scale of the bridge. Move the cell up and
down in the solution several times and repeat the measurement 68. Apparatus
until successive readings are constant. 68.1 A medium-size glass Soxhlet extraction apparatus
62.5 Before each measurement rinse the cell thoroughly in provided with a siphon chamber approximately 35 mm diam-
reagent water and gently shake off any water clinging to the eter and 90 mm high. Alternatively, use a modified extraction
surfaces. apparatus of similar size equipped with a siphon cup to hold the
62.6 Blank—Correct the conductivity of the extract solu- thimble.
tions for the blank error. Determine this correction by running 68.2 Thimble, Alundum or paper, or some other inert device
a blank in parallel with the actual determination, using the to prevent fiber being carried over into the flask.
same volume of reagent water. 68.3 Heating Apparatus—Steam bath or variable tempera-
62.7 Test at least two specimens. If the conductivities on ture hot plates.
duplicate specimens do not agree within 10 %, repeat the 68.4 Evaporation Facilities.
determination.
69. Reagent
62.8 For referee purposes, condition the specimen and
weigh at the standard test conditions specified in Section 15. 69.1 Solvent, of specified composition.
70. Test Specimen
63. Calculation and Report
70.1 From the sample obtained in accordance with Sections
63.1 Calculation—Calculate the conductivity of the extract 6 to 13, cut a composite test specimen, weighing at least 25 g,
solution (based on the weight of 1 g of the air-dry sample) as into small pieces approximately 10 mm (0.4 in.) square, and
follows: mix thoroughly. Determine the moisture content in accordance
Conductivity 5 @~K/R2! 2 ~K/R 3!# 3 10 6 µS/cm (9) with 38.1 on a separate portion of the composite specimen in
moisture equilibrium with the portion for analysis.
where:
K = cell constant (C 3 R), cm−1, 71. Procedure
R 2 = resistance of extract solution at 25 6 0.5°C, V, and 71.1 Warning: The solvents used are likely to be flammable
R3 = resistance of water blank at 25 6 0.5°C, V. and may be physiologically hazardous. Take appropriate pre-
63.2 Report—Report in accordance with Section 14. cautions to prevent ignition and to reduce exposure to the
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D 202 – 97 (2002)e1
liquids and their vapors to below the maximum safe levels. planned to develop such a statement.
71.2 Heat the flask to constant weight in an oven at 105 to 73.2 This procedure has no bias because the value of
110°C, allow to cool in a desiccator, and weigh to the nearest solvent-soluble matter is defined in terms of this test method.
1 mg.
71.3 Place not less than 5 g of the specimen (weighed to the FIBER ANALYSIS
nearest 0.01 g) in the fiber-retaining device (thimble), that was
previously extracted with the solvent being used or tested to
show there is no contribution to the test from this source. 74.1 A fiber analysis consists of identifications of the kinds
71.4 Place the thimble in the extraction apparatus and add and types of fiber in a paper and determination of the
sufficient solvent so that a safe excess will remain in the bottom proportions in which they are present.
74.2 The results are reported as percentages by weight of
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of the flask when the siphon cup is full.

71.5 Place the assembled apparatus on the hot plate with the the total fiber composition to the nearest multiple of 5. When
heat adjusted so that siphoning occurs no more than once every any fiber is found present in amounts less than 21⁄2 % it is
6 min. At the end of the extraction, at least 60 times unless reported as a “trace.”
otherwise specified, (Note 15), pour the solvent from the
siphon cup into the flask. 75. Significance and Use
75.1 Fiber analysis is useful as a specification and a control
NOTE 15—When extracting with a solvent with a large heat of
test. It may be used in referee or research testing to determine
vaporization, such as water, the heating should be adjusted so that
siphoning occurs at least once every 10 to 12 min. In this case end the conformance to specification or purchase requirements con-
extraction at 36 siphonings. For the “medium” Soxhlet apparatus to siphon cerning fiber composition. For accurate results the analyst
properly with water, it may be necessary to have the siphon tube replaced needs considerable training and experience; needs to make
with one of larger internal diameter. Alternatively, the “large” (123 by frequent use of standard papers of known composition; needs
43-mm thimble) size of Soxhlet extraction apparatus usually is satisfac- to make frequent use of known samples of fiber; and to be
tory. thoroughly familiar with the reactions of different fibers to
71.6 Dry the previously tared flask on the heating apparatus, exposure to various stains.
using solvent recovery if desired, and then dry to constant
weight in an oven at 105 to 110°C. Allow to cool in a 76. Procedure
desiccator, and weigh to the nearest 1 mg. (Note that static may 76.1 Determine the fiber analysis in accordance with Test
be a problem in these weighings, and take steps to ensure the Method D 1030, except sample the material in accordance with
correct weight is obtained.) Sections 6 to 13 of these test methods.
71.7 Alternatively, evaporate the solvent from a tared
evaporating vessel, taking care to rinse the flask into the dish; 77. Report
in which case, taring of the flask as specified in 71.2 is not 77.1 Report in accordance with Section 14 and with Test
required. Method D 1030.
71.8 Test at least two specimens.
ABSORPTION (Rise of Water)
72. Calculation and Report
72.1 Calculation: 78. Significance and Use
72.1.1 Calculate the solvent-extractable content on the basis 78.1 The rise of water, which has a fixed surface tension,
of the oven dry weight of the specimen as follows: reflects a combination of conditions within the paper, including
A 5 100R/@W~1.0 2 0.01 M!#% (10) fiber arrangement, fiber size, spacing between fibers, specific
surface area of the fibers, and the presence, if any, of chemical
where: treatment of the paper fibers during or subsequent to manufac-
A = solvent extracted material, %, ture of the paper.
R = weight of residue, g,
78.2 This test method is useful for control purposes as one
W = original weight of specimen, g, and
M = moisture in the specimen, %. criterion of uniformity.
72.1.2 The test result is the average of the values calculated 78.3 With caution, this test may be used as an indicator of
in 72.1.1 for all specimens. impregnation rate.
72.2 Report in accordance with Section 14, and include the 79. Apparatus (see Fig. 3)
following information:
72.2.1 Previous treatment the sample may have had, for 79.1 Container.
example, previous extraction with another solvent, 79.2 Support for test specimens and scale.
72.2.2 Solvent used, and 79.3 Linear scale.
72.2.3 Time of extraction and approximate number of si- 80. Test Specimens
phonings.
80.1 Cut ten test specimens, 25 mm (1 in.) in width and at
73. Precision and Bias least 125 mm (5 in.) in length, from the samples obtained in
73.1 This test method has been in use for many years, but no accordance with Sections 6 to 13, five being cut parallel with
statement for precision has been made and no activity is the machine direction of the paper and five cut parallel with

D 202 – 97 (2002)e1
to penetrate through the paper is measured, and recorded as the
impregnation time. The endpoint is determined by visual
observation.
86.1 Impregnation time of a paper, using a standard liquid,
may be used to predict the rapidity and degree of impregnation
that may be obtained in commercial impregnation of this paper
with suitable liquids.
86.2 Where castor oil is used as the testing liquid, the
impregnation time has been shown to correlate with the rate of
commercial impregnation with phenolic resin varnishes. For
phenolic laminates, the impregnation time of the base paper is
an important factor affecting the strength, moisture-resistance,
and electrical properties of the finished laminated product.
86.3 This test method is also used in selection of cable
paper; for such use it is usually desirable to use the commercial
impregnant in the instrument.
87. Apparatus
87.1 Penetration Tester—A Williams standard tilting-type
penetration tester with orifice 60 mm (2.375 in.) in diameter as
FIG. 3 Apparatus for Absorption Test shown in Fig. 4, or equivalent penetrometer, equipped with a
stop clock graduated in seconds.
87.2 Thermometer—A thermometer of suitable range.
cross-machine direction of the paper. Condition the specimens 87.3 Test Liquid—Double-pressed castor oil having a vis-
as prescribed in Section 15. cosity of 700 6 30 cP (0.7 6 0.03 Pa·s) at 25°C (77°F), or
mineral oils of the same viscosity and comparable wetting
81. Procedure
characteristics are most commonly used as the test liquid.
81.1 Suspend the specimens vertically, with one end dipping However, other liquids which are more specific to the intended
3 mm (1⁄8 in.) in reagent water at room temperature, and after application for the paper may be used, if specified. The liquid
5 min note the rise of the water in the specimen above the level used must be defined in the test report.
of the water in the container. Measure the rise by reading the
height of absorption directly from the scale. Record the height 88. Test Specimens
of absorption to the nearest 3 mm for each direction for each 88.1 From samples obtained in accordance with Sections 5
specimen, and calculate the averages as the results. to 13, cut six test specimens 75 mm (3 in.) square. Condition
the specimens as prescribed in Section 15.
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82. Report
82.1 Report in accordance with Section 14. 89. Procedure
89.1 Measure the test specimens for thickness in accordance
83. Precision and Bias with Sections 16 to 3.
83.1 This test method has been in use for many years, but no 89.2 Number the test specimens consecutively on the same
statement for precision has been made and no activity is side of the paper. Test the odd-numbered specimens with their
planned to develop such a statement. numbered sides up, that is, not in contact with the impregnating
83.2 This test has no bias because the value for absorption liquid. Test the even-numbered specimens with their numbered
is defined in terms of this test method. sides down, that is, in contact with the impregnating liquid.
89.3 Place the liquid container in a horizontal position and
IMPREGNATION TIME fix the thermometer so that its bulb is immersed in the test
liquid. Fill the container with the impregnating liquid to within
84. Scope 6 mm (1⁄4 in.) of the upper edge of the container orifice.
84.1 This test method measures the time required for castor Maintain the liquid at this level by adding small amounts of the
oil, or another specified non-aqueous liquid, to penetrate impregnating liquid to replace that absorbed by the test
through the thickness of a paper, under specified conditions. specimens during the testing period. Maintain the temperature
of the liquid at 25 6 1.1°C (77 6 2°F) during testing by means
85. Summary of Test Method of the electrical heater and the thermostat in the base of the
85.1 A specimen of paper is clamped over an opening in the container.
top of a container filled with a designated liquid. The container 89.4 Place the specimen over the container orifice and
is then tilted so that the liquid is in contact with the bottom clamp in place with the ring clamp. After setting the stop clock
surface of the paper specimen. The time required for the liquid at zero, depress the container handle quickly until the front end

D 202 – 97 (2002)e1
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FIG. 4 Penetration Tester
of the container touches the base plate and start the clock. SURFACE FRICTION
Observe the surface of the paper closely and at the instant of
complete penetration of the liquid throughout the entire paper
area under test, stop the clock by immediately raising the front 92.1 The coefficient of dynamic friction of paper is a factor
end of the liquid container. in the satisfactory application of paper tapes used to insulate
conductors in electrical apparatus.
NOTE 16—It has been found that, for some liquids, particularly mineral 92.2 The sliding of one surface of paper over another paper
oils, the use of ultraviolet light is helpful in determining the “instant of
surface has been found to correlate with the frictional forces
complete penetration of the liquid throughout the entire paper area under
test”. that exist when paper surfaces slide over smooth metal surfaces
such as are encountered in high-speed tape winding equipment.
89.5 Record the elapsed time as the time of impregnation. 92.3 Paper-taped conductors may be bent during assembly
89.6 The average value for the six specimens is the test of electrical apparatus and it is desirable that the paper slide
result. upon itself when such bending is encountered.
90. Report 93. Apparatus
90.1 Report in accordance with Section 14, and include the 93.1 Inclined Plane (See Fig. 5)—constructed with a rigid
following information: smooth-surfaced flat material such as wood, plywood, or
90.1.1 Average impregnation time, decorative thermoset laminate, with the dimensions approxi-
90.1.2 Minimum and maximum impregnation times, or mately as shown in Fig. 5.
other indication of variance, 93.2 Mount the plane on a horizontal table.
90.1.3 Description of the test liquid, and 93.3 Equip the plane with a pointer to indicate the markings
90.1.4 Average, maximum, and minimum thickness before of the angle between the level table top and the inclined plane.
impregnation and the thicknesses of the specimens showing the Mark the scale to read angles to the nearest 1⁄4° with a
lowest and highest impregnation time. maximum angle of 30°.
93.4 Equip the plane with a mechanical linkage of gears and
91. Precision and Bias offset wheel or rack and pinion to raise the plane very slowly
91.1 This test method has been in use for many years, but no and smoothly during tests.
statement for precision has been made and no activity is 93.5 Make provisions on the plane to secure temporarily the
planned to develop such a statement. 200 mm (8 in.) wide test specimen to the plane surface. Bars
91.2 This procedure has no bias because the value of and wedges are useful for meeting this requirement.
impregnation time is defined in terms of this method. 93.6 Use an attached or portable leveling device to indicate

D 202 – 97 (2002)e1
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FIG. 5 Included Plane for Surface Friction Test
levelness of the plane in both dimensions at zero elevation. 94.5 The purchase order or specification for the material
93.7 Sliding Block—The sliding block (Fig. 6) of hardwood should indicate whether the test is to be made on the felt or
is 25 mm (1 in.) thick, 63 mm (21⁄2 in.) wide, and 75 mm (3 in.) wire side.
long with a smooth flat bearing surface and rounded edge and
with provisions for securing the ends of the paper specimen 95. Procedure
when it is wrapped around the flat sliding area. The block 95.1 Apply the test specimens to the inclined plane and
weighs 235 6 10 g. sliding block. It is important that the contact surfaces of the
paper specimens attached to the apparatus be smooth and free
94. Test Specimens of wrinkles.
94.1 Samples obtained in accordance with Sections 6 to 13 95.2 Gently place the block on the right back corner of the
must have particular attention paid to them. Take them from level plane, in position to slide. Place the block on the plane so
freshly exposed layers of paper and handle them so that they do that the rounded edge is on the downhill side of the incline.
not rub against one another or other objects, or become 95.3 By preliminary tests, determine approximately the
wrinkled or touched in any part of the area to be submitted to expected friction angle. Slowly raise the plane from 2° below
the friction test. that setting and at the same time gently tap the back edge of the
94.2 Condition all samples in accordance with Section 15. block. A pencil is a convenient tapping instrument.
94.3 Determine the wire side in accordance with TAPPI 95.4 The tapping should advance the block 3 to 6 mm (1⁄8 to
T455, and the machine direction in accordance with Test 1⁄4 in.) down the plane for each tap and be of a frequency that
Method D 528. Mark an arrow on one side of each specimen to at least one tap is registered for each 1⁄2° of rise of the
identify the wire side and the machine direction. adjustable inclined plane. The intensity of the taps to produce
94.4 For each test cut two test specimens 63 mm (21⁄2 in.) the desired motion of the sliding block will decrease as the
wide by 170 mm (7 in.) in the machine direction for use on the sliding block slides down the plane. Record the angle at which
sliding block. Cut one specimen 200 mm (8 in.) wide by 250 the block slides down the plane without further tapping as the
mm (10 in.) in the machine direction for use on the plane. If it preliminary test.
is specified that tests be made in the cross-machine direction 95.5 Take the second 63 by 170 mm specimen and attach it
change the direction of cutting appropriately. to the block. Place the block on the front half of the strip on the
FIG. 6 Sliding Block for Surface Friction Test

D 202 – 97 (2002)e1
inclined plane and repeat the procedure described in 95.3 and BURSTING STRENGTH
95.4, except raise the inclined plane to an angle 1° less than the
angle obtained in the preliminary test. The angle at which the 102. Scope
block slides down the plane without further tapping is the final 102.1 This test method describes two procedures for mea-
surface friction angle of the specimen. Record this angle to the suring the bursting strength of paper. One procedure applies to
nearest 1⁄4°. papers bursting up to 1.4 MPa (200 psi) and the second
95.6 Make three tests from each sample, unless the material procedure applies to papers bursting at values above this level.
specification requires a different number. The average value of
all tests is the test result. 103. Summary of Test Method
103.1 A conditioned specimen of paper is clamped between
96. Report two flat surfaces that have circular openings of a specified
96.1 Report in accordance with Section 14. If desired, the diameter and edge shape. A rubber diaphragm is pressed
test results may be reported as dynamic coefficient of friction against one surface of the specimen with steadily-increasing
by determining the tangent of the surface friction angle. hydraulic pressure until the specimen ruptures. The hydraulic
pressure at the moment of rupture is the test value.
97.1 This test method has been in use for many years, but no 104. Significance and Use
statement for precision has been made, and no activity is 104.1 Bursting strength has considerable use as a mill
planned to develop such a statement. control test and, to some extent, as a purchase specification
97.2 This test method has no bias because the value for requirement.
surface friction is defined in terms of this method. 104.2 It is not easy to identify applications for electrical
insulating paper in which forces are normally encountered that
AIR RESISTANCE duplicate the forces exerted in this test method. For this reason
there is controversy among experts regarding the significance
98. Scope of this test when applied to electrical insulating papers.
98.1 These test methods provide three procedures for the
determination of the air resistance of paper. While they are 105. Test Specimen
similar in principle, the procedures are intended for different 105.1 Prepare specimens from the sample obtained in ac-
ranges of porosities, and the results obtained using one method cordance with Sections 6 to 13, and conditioned in accordance
cannot be compared directly with those obtained by another with Section 15.
test method. 105.2 For each test, allow at least a 100 mm (4 in.) square
area.
99. Significance and Use 105.3 If practicable, cut sufficient material to permit ten
99.1 Air resistance is related to dielectric strength and bursting tests on a straight line across the sheet or roll.
absorbancy, and thus may be used as a criterion in specifica-
tions for insulating papers, while recognizing that the values 106. Procedure
obtained may vary over a considerable range even on paper of 106.1 Procedure A (for papers bursting up to 1.4 MPa (200
quite uniform formation. psi)—Determine the bursting strength in accordance with Test
99.2 Air resistance reflects the internal structure and surface Method D 774, except sample and condition the material in
condition of the paper: differences in the types of fibers, in their accordance with Sections 6 to 13 of these test methods.
degree of hydration, length, orientation, and compaction, in the 106.2 Procedure B (for papers bursting at more than 1.4
amount or nature of noncellulosic additives, or in surface MPa);
treatment. 106.2.1 Apparatus for Procedure B is a testing machine
conforming to the following requirements:
100. Procedure 106.2.1.1 Clamps, similar in all respects to those used on the
100.1 Determine air resistance in accordance with Method machine specified in Test Method D 774.
A, B, or C of Test Methods D 726, except sample the material 106.2.1.2 Rubber Diaphragm made of pure gum rubber,
in accordance with Sections 6 to 13 herein. free of mineral loading material, and conforming to dimensions
100.2 Select the test method most suitable for use on the of Fig. 7.
paper being tested, as discussed in Test Methods D 726. It is 106.2.1.3 Motor—The hydrostatic pressure applied to the
recommended that the test method to be used be given in the underside of the rubber diaphragm until the test specimen
specification for the paper being tested. bursts shall be generated by a motor-driven piston forcing a
liquid (usually glycerin or hydraulic brake fluid) into the
101. Report pressure chamber of the apparatus at the rate of 170 6 10
101.1 Report in accordance with Section 14, and also mL/min (10.4 6 0.6 in.3/min).
include the following information: 106.2.1.4 Pressure Reading Gages—The pressure reading
101.1.1 A statement as to which test method was used, and gages shall indicate the bursting strength in megapascals (or
101.1.2 Information specified in the pertinent report section pounds force per square inch) with the following minimum
of Test Methods D 726. accuracy:
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D 202 – 97 (2002)e1
condition in accordance with Section 15 herein.
109.2 Determine the folding endurance in accordance with
Test Method D 2176, which is the preferred method; or TAPPI
T 423. If TAPPI T 423 is used, it must be so stated in the
report.
NOTE 17—The test results obtained using Test Method D 2176 will in
general differ greatly from those using TAPPI 423. The difference between
the two values will depend upon the applied tensile forces, the grade of
paper being tested, and other factors, so that no direct comparison can be
made between papers tested by different methods.
110. Report
110.1 Report in accordance with Section 14, and the Report
section of Method D 2176 or TAPPI T 423, as applicable, and
identify the procedure used.
TENSILE PROPERTIES
111. Scope
111.1 This test method covers the determination of three
tensile breaking properties of paper, namely; the energy ab-
sorbed per unit of surface area (tensile energy absorption), the
force per unit cross-sectional area or per unit width required to
break a specimen (tensile strength), and the percentage elon-
gation at break.
111.2 This test method is applicable to all types of paper
FIG. 7 Rubber Diaphragm for Bursting Strength whose properties are within the working range of the instru-
ment used.
Pressure Accuracy
MPa psi MPa psi 112. Summary of Test Method
0 to 2.1 0 to 300 0.02 3.0
0 to 4.1 0 to 600 0.04 6.0 112.1 Conditioned test specimens having smooth, straight
0 to 6.9 0 to 1000 0.07 10.0
Above 6.9 Above 1000 0.14 20.0
parallel edges are subjected to tensile stress, uniformly across
the width of the specimen, under specified conditions of
106.2.2 Procedure—Make ten bursts, as in 106.1, using loading.
apparatus as described for Procedure A or Procedure B, as 112.2 Depending upon which properties are of interest, the
applicable, five with one side of the specimen uppermost and stress (load) at rupture, the strain (elongation) at break, or the
five with the other side uppermost. Operate the testing machine area (in units of work) under the stress-strain curve are
at a uniform speed until the specimen bursts. measured for use in calculating the specified properties.
107. Report 113. Significance and Use
107.1 Report in accordance with Section 14. 113.1 Tensile strength is an indication of the suitability of
FOLDING ENDURANCE papers for applications where, during manufacture or in ser-
vice, direct tensile stresses are applied to tapes or sheets of the
108. Significance and Use paper.
108.1 Folding endurance of paper is a measure of its 113.2 The elongation at break is useful in predicting the
toughness and brittleness, that is, the tendency for the fibrous performance of a paper when applied by machines in the
structure to pull apart or for the fibers themselves to break in manufacture of coils, capacitors, insulated conductors, etc.
two. Since folding endurance is very sensitive to changes in Such machinery may subject paper to severe tensile stresses,
several of the other physical properties of paper, it is a very and the elongation at rupture has been found to correlate with
useful criterion for determining the extent of changes such as runnability on such machinery. This property is also valuable in
occur in the heat stability test. evaluating a paper that is required to conform closely to an
108.2 Either of the test methods specified in Section 109 irregular surface. In the case of creped papers, it is frequently
may be used for the determination of the effect of heat aging the property of primary interest.
(Sections 131 to 137), since relative values only are involved. 113.3 The tensile energy absorption (TEA) measures the
For specification purposes, however, the use of Test Method ability of the paper to withstand shock or impact. It is
D 2176 is strongly recommended. indicative of the suitability of the paper for use on machines
where it may be subjected to tensile impact, and for applica-
109. Procedure tions where such forces are applied in service.
109.1 Sample in accordance with Sections 6 to 13 and 113.4 All three tensile properties are influenced by:
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D 202 – 97 (2002)e1
113.4.1 The kind, quality, and treatment of the paper fibers,
113.4.2 The kind and amount of non-fibrous constituents of
the paper,
113.4.3 The formation of the sheet on the paper-making
machine,
113.4.4 Subsequent drying, finishing and treatment of the
paper,
113.4.5 Exposure of the paper to severe environments,
including high temperature, high humidity, or other degrading
factors, and
113.4.6 Moisture content at time of testing.
113.5 Values for all of the tensile properties are useful for
material specifications, for process control, and for research.
114. Apparatus
114.1 Tensile Testing Machine, having the following char-
acteristics:
114.1.1 Capable of applying a tensile load in a predeter-
mined manner, smoothly and reproducibly, using suitable jaws
(see 114.2) to clamp the test specimen.
114.1.2 Means for indicating the applied load at break with
an accuracy of 61 % of the load at break, at the loading rate
used for the test,
114.1.3 Means for determining elongation of the test speci- FIG. 8 Modified Line Clamp Jaws for Scott A-1 Clamp
men at the time of break to an accuracy of 60.05 % of the
initial test span, and
114.1.4 Means for recording the applied load and the 114.3 Planimeter, for determination of the area under the
elongation of the test specimen, without loss of accuracy, load-elongation curve, with an accuracy of 61 %.
continuously from initial application of load until the time of 114.3.1 Alternatively, the recorder may be equipped with an
failure. automatic integrator having the same accuracy.
114.3.2 If neither a planimeter nor an integrator is available,
NOTE 18—The recorder specified in 114.1.4 may not be needed if TEA the area under the curve may be determined by cutting the
is not being measured. Also if only tensile strength is of interest, the load
recorder paper along the curve, the elongation axis, and the line
at break will be the only reading of significance.
NOTE 19—Tensile testing machines of both the constant-rate-of- representing the elongation at rupture. The weight of this piece
extension (CRE) and pendulum type are commonly used for measuring of paper and the weight of a rectangular section from the same
tensile properties of paper. CRE machines are almost universally used for piece of paper, and having an area of at least two-thirds that of
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determining TEA. Results obtained on one type of machine may not the area under the curve, may then be determined on an
conform closely to results obtained on duplicate specimens tested on a analytical balance, and the area under the curve calculated.
machine of the other type. 114.4 Specimen Cutter, for preparing specimens meeting
114.2 Clamping Jaws, for gripping the ends of the test the requirements of 115.3.
specimen. 114.5 Scale and Magnifier, or Optical Comparator, accurate
114.2.1 The clamping surfaces shall be in the same plane, to the nearest 0.1 mm (0.004 in.), for measuring the width of
parallel to the direction of motion of the moving jaw. The jaws specimens.
shall be at least as wide as the test specimen, with the edges of
the clamping surfaces perpendicular to the edges of the test 115. Test Specimens
specimen. 115.1 Prepare test specimens from samples taken in accor-
114.2.2 Creped papers, which tend to slip in the jaws of dance with Sections 6 to 13, and conditioned in accordance
conventional flat-faced clamps, may be tested using line with Section 15. Store and test prepared specimens in a
clamps of the type shown in Fig. 8, whereby the specimen is standard laboratory atmosphere as specified in Section 15.
clamped between a sharp ridge on one jaw and a reinforced 115.2 Prepare sufficient specimens to obtain ten valid tests
rubber mat on the other. Use a cloth-inserted rubber sheet in each of the principal directions of interest. Because of the
packing 3 mm (1⁄8in.) thick16 for covering the flat jaw. When possibility of some test values being rejected for reasons as
using jaws of this type, the initial separation is the distance given in 117.6, it is advisable to prepare a few extra specimens.
between the ridges on the jaws at the time tension is first 115.3 Cut the test specimens with clean straight parallel
applied. edges to a width of within 0.1 mm (0.004 in.) of the specified
width, and of a length sufficient to permit clamping the
specimens in the jaws at the specified initial span, without the
16
Raybestos-Manhattan 645 Rubber Diaphragm Sheets have been found satis- necessity for touching the portion of the specimen that will be
factory for this method. between the jaws. If the width of the specimens cannot be held

D 202 – 97 (2002)e1
within 0.1 mm of the specified width, measure and record the NOTE 22—Ordinarily, the tensile strength is expressed in stress per unit
width of each specimen to an accuracy of 60.1 mm. In all width for papers up to 0.25 mm (0.010 in.) or even greater in thickness.
cases, the edges of the specimens must be straight and parallel For thinner papers, a decision to require determination and reporting of
tensile strength in units of force per unit cross-sectional area should be
with the variation in width of any specimen not exceeding 0.1 made only after considering the effect that errors in measuring thickness
mm. The specimen width must in any case be within 1.0 mm will have on the accuracy of the calculated test results.
(0.040 in.) of the specified width.
115.4 The recommended specimen widths and the initial 117.3 Set the span between the jaws to the proper distance,
test spans are as follows: as given in 115.4, or as may be otherwise specified for the
Condition Width Span
material being tested. The test span shall be within 5 % of the
Measurement of TEA, and simultaneous de- 25 mm (1 in.) 200 mm (8 in.) specified distance and shall not vary over a range of more than
termination of tensile strength and elongation 1 % of the distance specified during the testing of any group of
at break.
Measurement of tensile strength and elonga- 15 mm (0.6 in.) 180 mm (7 in.)
test specimens. The actual span shall be known with an
tion at break on uncreped papers accuracy of 60.5 % if TEA or elongation at break is to be
Measurement of tensile strength and elonga- 25 mm (1 in.) See Note 20 determined.
tion at break on creped papers.
117.4 Align a test specimen in the two sets of jaws and
NOTE 20—For creped papers, the most suitable test span is a function clamp it in the upper set of jaws.
of the expected elongation at break, and the test span to be used should be 117.4.1 Remove slack from the specimen and align it by
specified in the document calling for this test method, or otherwise agreed
putting a small tension on it while clamping it in the lower set
upon between all parties concerned with the tests. Suggested test spans
are: of jaws.
Expected Elongation, % Test Span, mm (in.)
117.4.2 Use a clamping pressure sufficient to prevent slip-
0 to 50 180 or 200 (7 or 8) page during test without damaging the specimen.
51 to 100 100 (4)
101 to 200 50 (2) NOTE 23—Except for a referee test, time may be saved, when testing
201 to 400 25 (1) thinner papers, by aligning and clamping the ends of the ten specimens
Some pendulum-type testers may not have sufficient travel to permit testing together in the upper jaws, and breaking them one at a time, after clamping
with specimens of these lengths. If such instruments are to be used, it may be the lower end of each in the lower jaws.
necessary to agree to use shorter test spans for some grades of paper. NOTE 24—Some test machines operate with the lengthwise center line
115.5 In all cases the specimens shall be between 13 mm of the test specimen in a horizontal plane rather than in a vertical plane.
For these machines, the phrases “upper jaws” and “lower jaws” in the
(0.5 in.) and 50 mm (2.0 in.) in width.
preceding and subsequent sections shall be appropriately modified to
NOTE 21—In general, varying the width of the test specimen within this accommodate the peculiarities of these machines.
range has little effect on the test results for the papers normally used for
electrical insulation. However, this assumption should be verified by
117.5 Operate the test machine to apply stress to the
actual tests on the papers under consideration before placing reliance on specimen and break it.
it. 117.5.1 Except as noted below or in the specification for the
115.6 Cut the test specimens from areas of the sample which material under test, operate the tester at a speed such that the
--`,,,`,`,`,`````,,,```,,`,,`,`-`-`,,`,,`,`,,`---
are free of abnormalities, creases, or wrinkles, unless such average time from initial application of load to break is 5 to 15
defects are typical of the material being tested, or unless the s for any set of ten specimens. For referee tests, the average
purpose of the test is to determine the effect of such abnor- time to break shall be 8 to 12 s.
malities. 117.5.2 Most pendulum-type machines operate at a single
traverse rate of 300 mm/min (12 in./min), or at a small number
116. Calibration of fixed speeds, usually including 300 mm/min. The average
116.1 Calibrate the testing machine in accordance with the time to break and the traverse speed should be noted when this
manufacturer’s instructions and with Specification D 76 and type of machine is used.
Practices E 4. 117.5.3 When determining TEA on a CRE machine, use a
116.2 Calibrate the planimeter or other area measuring speed of 25 6 5 mm/min (1.0 6 0.2 in./min), when using a 200
equipment in accordance with the manufacturer’s instructions. mm (8 in.) test span. For other test spans, adjust the speed
116.3 Calibrate the scale or comparator in accordance with proportionally to give the same straining rate.
Practice D 2865. 117.5.4 In selecting the proper speed, as indicated in 117.5.3
or as specified in the document calling for this test method, the
117. Procedure maximum speed that can accurately be used on a given
117.1 Determine the width of the specimens to within 0.1 machine is determined in part by the response time of the
mm (0.004 in.). Discard specimens whose width is not uniform devices for indicating and recording load and elongation. The
within 0.1 mm over their entire length. While making this rate of increase of load or of elongation must be low enough
measurement and in all other steps until the specimen is that errors at any point on the curve due to lag in the indicating
broken, take care to avoid touching the test specimen with the or recording devices will be less than 1 % of the values at
fingers in the area which will be between the jaws, or otherwise break. In general full-scale response time should be less than 5
damaging or contaminating the specimen in the test area. s in either direction. See Specification D 76 for further discus-
117.2 If the tensile strength is to be reported in stress per sion of this subject.
unit of cross-sectional area, determine the thickness of each 117.6 Reject readings from individual specimens that slip in
specimen to within 0.01 mm (0.0005 in.). the jaws or break in or at the edge of the jaws. Slippage is

D 202 – 97 (2002)e1
usually caused by low clamping pressure. Jaw breaks may be 120. Precision and Bias17,18
caused by excessive clamping pressure, sharp jaw edges, or 120.1 Precision:
uneven stresses. 120.1.1 Interlaboratory tests indicate that two test results,
117.7 Record the values for load at break and for elongation each representing an average of ten determinations, from the
at break. The point of break is that of maximum applied load. same or different samples as noted, can be expected to agree
If possible, select scales for indicating or recording load and within the amounts as follows (95 % probability):
elongation such that the values at break are within the upper Tensile
Elongation TEA
half of the scale, and, in any case, to give the accuracies Strength
Repeatability (same sample, operator and 5 9 10 to 16
specified in 114.1. apparatus),%A
117.8 Determine the area enclosed by the load-elongation Comparability (samples markedly different in 9 16 15 to 16
other properties, but not in designated prop-
curve, the elongation axis and the line representing elongation erty, same operator and apparatus),%A
at break, using a planimeter, or alternate equipment as de- Reproducibility (same sample, different labo- 10 25 22 to 36
scribed in 114.3. ratories), %A
A
Percentage of the average of the two test results.
118. Calculation 120.1.2 In each case, the coefficient of variation of a test

result (average of 10 determinations) is expected to be about
118.1 For each test specimen calculate: 0.36 times the value shown in 120.1.1.
118.1.1 Tensile strength, either in force per unit width of 120.1.3 The information in 120.1.1 is based on tests made
specimen (kN/m or lb/in.), or in force per unit cross-sectional on papers having elongation of 10 % or less. The validity of
area of specimen (kPa or psi). these figures for papers of greater elongation has not been
118.1.2 Elongation at break, expressed as a percentage of determined.
the span at initial application of load. 120.2 Bias—A statement of bias cannot be made due to the
118.1.3 Multiply the integrator or planimeter value by the lack of a standard reference material.
appropriate factor for the equipment and settings to obtain the INTERNAL-TEARING RESISTANCE
area under the load elongation curve. Calculate the tensile
energy absorption according to one of the following equations: 121. Scope
TEA 5 10 6 A/LW J/m2 (11) 121.1 This test method covers the determination of the
TEA 5 12 a/lw lbf•ft/ft 2 (12)
average force in grams required to tear a single sheet of paper
after the tear has been started.
where: 121.2 This test method is not suitable for determining the
TEA = tensile energy absorption, J/m2 or lbf·ft/ft2 cross-directional tearing resistance of papers having tensile
A = area under load-elongation curve, J, strength in the machine direction that is much higher than in
L = initial test span, mm, the cross-machine direction.
W = specimen width, mm,
a = area under load-elongation curve, lbf·in., 122. Summary of Test Method
l = initial test span, in.,
122.1 A pendulum is permitted to make one swing and
w = specimen width, in., and 1 J/m2 = 0.0685 lb·ft/ft 2.
thereby cause the tearing of one or more sheets together
through a fixed distance. The work done in tearing is measured
118.2 For each set of test specimens calculate the averages by the loss in potential energy of the pendulum. The scale is
for tensile strength, elongation at break, and TEA; and deter- calibrated to indicate average force (work done divided by
mine the range, standard deviation, or other indication of tearing distance).
variability.
119. Report 123.1 The results of the test are suitable for the following:
119.1 Report in accordance with Section 14, and include the 123.1.1 For acceptance; process control; research; or referee
following information: testing, and
119.1.1 Average value and indication of variability for 123.1.2 For measuring serviceability (suitability) of papers
tensile strength, elongation at break, and TEA, as calculated in which in use are subjected to tear strain.
Section 118, 123.2 Tearing resistance of paper is influenced by:
123.2.1 The kind, quality, and treatment of the paper fibers,
119.1.2 Type of testing machine used,
123.2.2 The formation of the sheet on the paper-making
119.1.3 Rate of loading, machine, and
119.1.4 Average time to break,
119.1.5 Width of test specimens,
17
119.1.6 Initial test span, and Lashof, T. W., “Precision of Methods for Measuring Tensile Strength, Stretch
and Tensile Energy Absorption of Paper,” TAPPI Vol 46, January 1963, pp. 52–59.
119.1.7 Number of individual tests rejected, and the reasons 18
Data in Section 120 were abstracted from TAPPI T-494, Tensile Breaking
for rejection. Properties of Paper and Paperboard.
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D 202 – 97 (2002)e1
123.2.3 The treatment of the sheet after formation (includ- 130.1.2 For some grades of papers (three of the five tested),
ing machine wet pressing and calendering). the use of two different stirrups, even by the same laboratory,
produced values that were, with 95 % confidence, significantly
124. Procedure different.
124.1 Determine the tearing resistance in accordance with 130.1.3 At the 95 % confidence level, there was no signifi-
Test Method D 689 or TAPPI T 414, except sample the cant difference between the results obtained on the pendulum-
material in accordance with Sections 6 to 13 of these test type and on the constant-rate-of-extension machines.
methods, and use the minimum number of sheets necessary to 130.2 This method has no bias because the value for
bring 80 % of the test measurements above 20, the minimum edge-tearing resistance is defined in terms of the method.
permissible scale reading.
HEAT STABILITY IN AIR
125. Report 131. Scope
125.1 Report in accordance with Section 14 and with Test 131.1 This test method determines the retention of one or
Method D 689 or TAPPI T 414. more selected properties of a paper sample when test speci-
mens are subjected to a specified period of heating in air at
EDGE-TEARING RESISTANCE
120°C.
126. Scope 132. Significance and Use
126.1 This test method covers the determination of the 132.1 During the fabrication of electrical equipment in
edge-tearing resistance of electrical papers. A strip of paper is which electrical insulating paper is a component, the paper
folded around the edge of a shallow V-notch in a thin beam and may be exposed to air at elevated temperature. This heat
pulled to tear the paper at the edges. A standard testing machine stability test evaluates the effect of such exposure upon the
is used to apply and measure the force required to cause physical characteristics of the paper. Results of this test method
tearing. are suitable for production control, for routine acceptance
testing, and for research.
132.2 Heat stability in air, as measured by this test method,
127.1 For certain manufacturing operations such as high- does not evaluate the “life”, “thermal aging”, or suitability of
speed wire wrapping, the edge-tearing resistance may correlate a paper for use at elevated temperatures. More complex
well with performance of a given paper. methods are required to evaluate such characteristics.
127.2 When comparing papers whose properties other than
edge-tearing resistance differ greatly, it is generally not accu- 133. Apparatus
rate to predict the relative performances of the papers solely on 133.1 Baking Oven—An electrically heated oven.
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the basis of their edge-tearing resistances. Other properties, 133.2 Specimen Holding Fixture—A fixture for holding the
such as tensile strength, elongation, internal tearing resistance, specimens while in the oven. The fixture must be of appropriate
surface friction, and directionality may also affect the perfor- dimensions for holding the specimens and keeping them
mance of a given paper. separated and protected from damage during exposure to
heating in the oven.
128. Procedure 133.3 Testing Equipment—There must be suitable test
128.1 Determine the edge-tearing resistance in accordance equipment for each property by which heat stability is to be
with Test Method D 827 or TAPPI T 470 except sample in evaluated. Depending on the intended use, evaluation may
accordance with Sections 6 to 13. reasonably be in terms of folding endurance (Sections 108 to
110), internal tearing resistance (Sections 121 to 125), edge
129. Report tearing resistance (Sections 126 to 130), tensile strength
129.1 Report in accordance with Section 14 and Test (Sections 111 to 120), elongation (Sections 111 to 120), tensile
Method D 827 or TAPPI T 470. energy absorption (Sections 111 to 120), bursting strength
(Sections 102 to 107), or a combination of properties.
134. Test Specimens
130.1 Precision—From a round-robin test19 involving five
laboratories each testing five grades of paper on two types of 134.1 Cut a sufficient number of test specimens in one or
machines, with a common stirrup used by all laboratories in both of the principal directions, as may be specified, from
addition to each one’s individual stirrups, the following con- samples obtained in accordance with Sections 6 to 13, in
clusions were drawn: dimensions to suit the chosen test or tests to be made. Divide
130.1.1 For papers having edge-tearing resistance between the test specimens into two similar sets, each composed of
18 N (4 lb) and 200 N (45 lb), the between-laboratory corresponding adjacent pieces as cut from the samples. One set
difference on specimens cut from the same sample of paper is for the baking treatment and subsequent tests, the other set
should not exceed 10 %. for comparative tests of unbaked specimens.
135. Procedure
19
Supporting data are available from ASTM Headquarters. Request RR:D-9- 135.1 Mount the specimens to be heat-treated on the fixture
1004. specified in 133.2.

D 202 – 97 (2002)e1
135.2 Place the specimens, in the holding fixture, into the 139.2.1 Method B permits location of the defects for repair
oven. Establish the period of baking such that at least one or removal, as may be desired.
variety of test specimen shall experience at least 20 % of loss 139.3 Conducting paths tests may be used for manufactur-
in the test. A 72-h period is usually sufficient for this require- ing control, or for acceptance evaluation.
ment.
135.3 Remove the baked specimens from the holding fix- 140. Sampling
ture, taking care not to damage them, and condition them in 140.1 Sample in accordance with Sections 6 to 13, and with
accordance with Section 15 before testing. Approach the consideration of the specimen requirements and capabilities of
conditions of testing for both the baked and the unbaked the test method.
specimens from a humidity lower than 50 % relative humidity
to avoid possible hysteresis effects. Test the conditioned Method A—For Papers 0.04 mm (0.0015 in.) and Under in
unbaked and baked specimens during the same test period. Thickness
135.4 Calculate the heat stability as 100 times the ratio of
141. Apparatus
the test result for the aged specimens to the corresponding test
result for the unaged specimens. 141.1 Electrodes—Two electrodes, consisting of a smoothly
machined cast iron or other metal plate, and a hand-operated
136. Report metal roller with smoothly machined face and fitted with an
136.1 Report in accordance with Section 14, and also insulated handle. The plate shall be of convenient size to
include the following information: accommodate the specimens to be tested. The finished dimen-
136.1.1 The time of baking, h, sions of the roller shall be as follows:
136.1.2 The property by which stability was measured, and mm in.
Diameter 50 2.0
the method used to determine that property, Width of face 25 1.0
136.1.3 Test results for the baked and unbaked specimens,
NOTE 25—For papers less than 38 mm (1.5 in.) wide use a roller with
and
a face width of 10 mm (0.37 in.).
136.1.4 Calculated heat stability, %.
141.2 Detector—An impulse counter or loud speaker hav-
137. Precision and Bias ing a resistance of 3000 V.
137.1 The precision of this test method has not been 141.3 Resistor, 80 000 V.
determined, and no activity is planned to determine its preci- 141.4 Voltage Supply—A source of 110 V dc, with one
sion. terminal grounded.
137.2 This test method has no bias because the value for 141.5 Circuit—Connect the detector in series between the
heat stability is defined in terms of the method. plate electrode and the grounded terminal of the voltage
supply. Connect the resistor in series between the roller
CONDUCTING PATHS electrode and the 110-V terminal of the voltage supply.
138. Scope 142. Test Specimen

138.1 These test methods provide procedures for testing 142.1 The test specimen, of sufficient size to cover the plate
electrical insulating paper for the presence of localized areas electrode, shall be held in place by weights. Test several such
that will conduct an electric current. Method A is limited to specimens. The paper must contain not more than 8 % moisture
papers not over 0.040 mm (0.0015 in.) thick. Method B is when tested.
limited to papers over 0.04 mm in thickness, since thinner 142.2 It has been found in the testing of thin papers that
paper might be damaged mechanically by the test. The upper great care must be taken in handling the specimens. They must
limit of thickness is self-determining at the greatest thickness not be touched with the hands nor should they be laid upon
that can be handled in a continuous web on the equipment. anything but the plate electrode after removal from the roll.
138.2 There are similarities between the tests described
herein and Test Method D 1389. The principal, and critical, 143. Procedure
difference with D1389 is that D1389 uses alternating voltages 143.1 Warning— High Voltage: Lethal voltages may be
for detecting conducting paths. present during these tests. It is essential that the test apparatus
and all associated equipment that may be electrically con-
139. Significance and Use nected to it be properly designed and installed for safe
139.1 Conducting paths seriously reduce the insulating operation. Solidly ground all metal parts that any person might
value of paper under electrical stress, and may result from come into contact with during the test. Thoroughly instruct all
either structural imperfections or inclusions. operators in the proper way to conduct the tests safely. When
139.1.1 The conducting paths count may reflect the relative making high voltage tests, particularly in compressed gas or in
cleanliness of the base pulp, the process water, the physical oil, the energy released at breakdown may be suffıcient to result
manufacturing system, or any combination thereof. in fire, explosion, or rupture of the test chamber. Design of test
139.2 The conducting paths tests indicate the frequency of equipment, test chambers, and test specimens should be such
occurrence of dielectric defects and facilitate isolation of areas as to minimize the possibility of such occurrences, and to
where they are excessive. eliminate the possibility of personal injury.
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D 202 – 97 (2002)e1
143.2 Secure the test specimen flat upon the plate electrode be raised above or lowered onto the plate surface, automati-
by means of weights at the ends. Turn on the voltage supply cally aligning the roller surfaces with the plate surface. The
and, when it is delivering 110 V, pass the roller once over rollers and plate shall be adequately insulated from each other.
parallel sections of the test specimen, carefully not overlap- The rollers shall be mounted so that continuity of electrical
ping, at a speed from 25 to 100 mm/s (1 to 4 in./s). Each connection between them and the potential source is assured
impulse recorded by the counter or heard as a click on the loud when they are rotating. The two rows of rollers shall be
speaker indicates a conducting path. mounted with their axes 90° to the direction in which the test
specimen is moved. The rollers in each row shall be spaced 35
144. Calculation
mm (13⁄8in.) apart on center lines, and the two rows shall be so
144.1 Calculate the number of conducting paths per unit placed that the midpoints of the rollers in one row are opposite
area as follows: the midpoints of the spaces in the other row as shown
Number of conducting paths per unit area 5 B/A (13) schematically in Fig. 9. The total weight exerted by each roller
on the surface of the specimen shall be not more than 315 g nor
where: less than 245 g.
B = total number of conducting paths determined on all
test specimens, and 146.2 Electrodes, Type 2—Two electrodes consisting of a
A = total area contacted by the roller. steel or other suitable metal roller, 150 mm (6 in.) or more in
diameter, and at least as wide as the width of the paper web to
145. Report be tested; and a flexible metal blade or blades. The blades shall
145.1 Report in accordance with Section 14, and include the be mounted in such a way that they may be pressed tangentially
number of conducting paths per unit area and the total area of against the roller electrode in a pattern wide enough to cover
paper tested. the entire width of the paper under test, with the exception of
such a margin as is needed at the edge to prevent the electrodes
Method B—For Papers Over 0.04 mm (0.0015 in.) in from coming in direct contact with one another, or to prevent
Thickness flashover between the electrodes.
146. Apparatus 146.2.1 The blade electrode may be a single blade designed
146.1 Electrodes, Type I—Two electrodes consisting of a to fit a given width of paper. It may also be two blades mounted
smoothly machined cast iron or other metal plate, and a set of in overlapping position which can be moved laterally to
smooth solid brass rollers. The plate dimension parallel to the provide an adjustable width, or it may be a series of narrow
direction over which the test specimen is moved shall be at blades mounted in a double row so that the midpoints of the
least 150 mm (6 in.); the other dimension of the plate shall be blades in one row are aligned with the midpoints of the spaces
at least as great as the width of the test specimen. between the blades in the other row. The individual blades shall
146.1.1 The surface of the rollers shall be machined and be wider than the open spaces between blades so that the entire
polished to smooth cylinders. The finished dimensions of the area of paper moving between the electrodes will be contacted
brass rollers shall be as follows: by at least one blade electrode in passage.
mm in.
146.3 Backstand—A stand upon which the roll of paper to
Diameter 38 1.5 be tested may be mounted with suitable tension controlling
Width of face 25 1.0 devices, such as are commonly used to control the unwind of
146.1.2 The rollers shall be mounted in two parallel rows paper.
above the plate electrode, and so arranged that each roller may 146.4 Winder—A takeup device which can draw the paper
FIG. 9 Arrangement of Brass Rollers Used in Surveying Medium Thick Papers for Conducting Paths (Method B)
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D 202 – 97 (2002)e1
from the roll through the electrodes and rewind it into a good 150. Report
roll, suitable for its intended use. 150.1 Report in accordance with Section 14, and include the
146.5 Voltage Source—A source of direct voltage which following information:
may be applied to the electrodes and varied to suit the 150.1.1 Number of paths per 100 m2 or 1000 ft 2, whichever
requirements of the paper under test. The voltage supply is applicable.
should be capable of delivering voltage up to the breakdown 150.1.2 Total area of paper tested,
level of the most resistant paper expected to be tested in the 150.1.3 Voltage applied, and
apparatus. 150.1.4 Running speed.
NOTE 26—Breakdown level in this case means the voltage at which
almost continuous discharge between the electrodes through the moving
web of paper is observed. 151.1 The precision of these test methods has not been
146.5.1 The voltage supply and collateral wiring should be determined, and no activity is planned to determine their
capable of handling an unknown but substantial current for a precisions.
short time when a conducting path passes between the elec- 151.2 These test methods have no bias because the values
trodes. for numbers of conducting paths are defined in terms of these
146.6 Detector—A signal or counting device that will methods.
indicate or record, or both, the momentary flow of current DIELECTRIC STRENGTH
when a conducting path passes between the electrodes. This
may be supplemented as desired by devices that will mark the 152. Scope
web at the approximate location of the conducting path. 152.1 The purpose of this test is to determine the dielectric
146.7 Measuring Device—A measuring wheel that contacts strength of untreated paper samples by the short-time test as
the moving web, attached to a suitable counter that will record described in Test Methods D 149.
the length of paper drawn through the electrodes. 152.2 Papers which have been subjected to treatments such
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147. Test Specimen as coating or impregnating with varnish may also be tested
using this test method. For papers to be tested after impregna-
147.1 Prepare the test specimen to whatever width is con- tion with a dielectric liquid, refer to Test Methods D 2413.
venient (usually the width of a commercial jumbo roll of paper)
and with a total area not less than 100 m2 or 1000 ft2 according 153. Significance and Use
to the units used in reporting the results of the test. The 153.1 This test, applied to untreated paper, may be used as
specimen may be an entire lot of paper rather than a sample a basis for determining uniformity in manufacture. It is suitable
selected to represent the lot. for use as a quality control, research, or specification test.
148. Procedure 153.2 This test method is suitable for the comparison of
148.1 Warning—See 143.1 for high-voltage warning. only those paper samples of similar thickness and apparent
148.2 Mount the rolled specimen on the backstand, pass the density.
end of it between the electrodes, and fasten it to a core on the 153.3 Refer to the Significance and Use section of Test
winder. Engage the measuring device and the detector. Apply Methods D 149 for further information on this subject.
voltage of a predetermined level to the electrodes. Start the 154. Apparatus
winder and draw the specimen through the electrodes at the 154.1 The apparatus shall conform to that specified in Test
predetermined speed. Record the number of conducting paths Methods D 149 using the Type 1 electrodes specified in Table
in the paper and the length of paper drawn through the 1 for sheet materials except that the upper 51 mm (2 in.)
electrodes. diameter electrode may be thicker than 25 mm (1 in.). This
148.3 The standard level of stress shall be direct voltage at upper electrode shall apply a load of 675 6 35 g to the
5.5 kV/mm (140 V/mil) of thickness. If any other level of specimen. For tapes, or sheet material to be compared with
voltage stress is used, it shall be upon agreement between tapes, the electrodes shall be 6 mm (0.25 in.) diameter rods as
purchaser and seller. specified as Type 3 in Table 1 of Test Methods D 149.
NOTE 27—It has been observed that the number of paths detected
increases with increase in voltage up to about 75 % of the breakdown 155. Test Specimens
level. 155.1 From the sample obtained in accordance with Sec-
148.4 There is no standard speed specified, as variation in tions 6 to 13, select specimens of sufficient area to provide for
speed has little or no effect on the number of conducting paths at least five tests. Condition the test specimens as prescribed in
detected when using direct voltage. Section 15 of these test methods. Make the dielectric tests in
the same standard atmosphere.
149. Calculation
149.1 Calculate, from the width of specimen and the re- 156. Procedure
corded length, the area of paper tested. From this area and the 156.1 Warning—See 143.1 for high-voltage warning.
recorded number of conducting paths, calculate the number of 156.2 Determine the dielectric strength in accordance with
conducting paths per 100 m 2 or 1000 ft2, whichever is the short-time test as described in Test Methods D 149 with the
applicable. following requirements:

D 202 – 97 (2002)e1
156.2.1 For paper with a total dielectric breakdown voltage 160.1.1 Dissipation Factor—The power loss in the dielec-
less than 2500 V, increase the voltage at a rate of 100 6 20 V/s. tric of ac equipment is important in their design and use. This
--`,,,`,`,`,`````,,,```,,`,,`,`-`-`,,`,,`,`,,`---
156.2.2 For paper having a total dielectric breakdown volt- loss has been found to be principally the result of dielectric
age between 2500 and 5000 V, increase the voltage at a rate of losses in the insulating paper of ac equipment such as capaci-
250 6 50 V/s. tors and power cables. Knowledge of the dissipation factor and
156.2.3 For paper having a total dielectric breakdown volt- its variation with temperature in insulating paper is important
age over 5000 V, increase the voltage at a rate of 500 6 100 in the design of paper-insulated electrical equipment. The
V/s. dissipation factor is a very sensitive measure of the purity of
156.2.4 In the case of a series of tests on the same batch of raw materials, of chemicals used in the manufacturing process,
specimens averaging about 2500 V or about 5000 V, make all and of cleanliness in the manufacturing process. The test is thus
such series of tests at the slower specified rate of voltage useful for quality-control purposes, subject to the interpretative
application. caution noted in 159.1.2.
156.2.5 From the average paper thickness for the sample, as 160.1.2 Permittivity—A value of permittivity which devi-
determined in Sections 16 to 24, calculate the kilovolts per ates significantly from that of similar papers measured under
millimetre or volts per mil for each puncture. comparable conditions suggests nonconformance of the speci-
156.3 In the case of papers that are very thin or very low in men to the electrode surface due to curl, wrinkles, folds, or
dielectric strength, use stacks of specimens as called for in the lumps within the specimen. Permittivity is also directly related
material specification or to effect a total minimum breakdown to the density of the paper, and may be affected by the addition
voltage of at least 600 V. of nonfibrous components.
157. Report 161. Apparatus

157.1 Report in accordance with Section 14 and the Report 161.1 Dissipation Factor and Capacitance Bridge—A
section of Test Methods D 149, and include the following guarded, high-voltage tape Schering bridge as described in Test
information: Methods D 150, or its equivalent, having an accuracy of
157.1.1 Number of thicknesses of paper tested if more than 60.0005 dissipation factor or 6 1 % whichever is greater, and
one, and a capacitance range from 50 to 1000 pF at 60 Hz.
157.1.2 Size and materials of construction of the electrodes. 161.2 Generator—A 60-Hz, 300-V or greater, generator.
Alternatively, voltage may be supplied from a 60-Hz line,
60-Hz DISSIPATION FACTOR AND PERMITTIVITY using a transformer and variable-ratio autotransformer.
OF DRY INSULATING PAPER 161.3 Detector—A detector having sufficient sensitivity to
provide a resolution in the dissipation factor balance of 2 3 10
158. Scope −5(0.00002) or 1 % of the reading, whichever is higher.
158.1 This test method covers the measurement of dissipa- 161.4 Electrodes—One or more sets of circular electrodes
tion factor and permittivity of dried, unimpregnated electrical with annular-guard electrodes constructed of a metal not
insulating paper. subject to distortion with repeated temperature cycling (See
Fig. 10). The electrode area shall be such that the capacitance
159. Summary of Test Method to be measured shall be within the range of the bridge. The gap
159.1 Dissipation factor and capacitance are measured on between measuring and guard electrodes shall be as small as
small specimens of paper held between precisely made elec- practicable, preferably no larger than the thickness of speci-
trodes and under prescribed pressures. The specimens thus held mens to be measured. A dead-weight pressure shall be applied
are dried under standardized conditions of heat and vacuum, to the specimen by addition of a known weight to the upper
then allowed to cool slowly in dry air while measurements of electrode. A total of 20 kPa (3.0 psi) is recommended for
dissipation factor and capacitance are made at a number of papers less than 0.04 mm (0.0015 in.) in thickness. The
temperatures. electrode surfaces shall be machined and lapped flat to within
159.1.1 The effective thickness of the specimen during 0.00125 mm (0.0005 in.) as determined by an optical flat. The
measurement may be determined by use of an auxiliary air-gap electrode surfaces shall be kept clean and shall be polished
capacitance measurement. Dissipation factor and capacitance periodically with crocus cloth to maintain flatness and smooth-
measurements of specimen and air gap, and calculation of ness.
permittivity, are made in accordance with methods described in 161.5 Vacuum Drying Equipment:
Test Methods D 150. 161.5.1 Vacuum Chamber—A vacuum chamber capable of
159.1.2 The complexity of the mixture of fibers and air being opened and resealed so as to be capable of evacuation to
comprising a sheet of paper requires that great care be taken in less than 2.7 Pa (20 µm Hg) under continuous pumping, and of
the measurement and interpretation of permittivity and dissi- being heated to at least 120°C. Electrical and temperature
pation factor. measurement connections shall be provided for measurements
within the chamber. The base plate shall be of suitable metal
160. Significance and Use and thickness (for example, ground cast iron) so that it will not
160.1 The general significance of dissipation factor and distort on repeated temperature cycling. Connections for
permittivity are stated in Test Methods D 150. With respect to evacuation and vacuum measurement, as well as electrical and
paper, the following also apply: temperature-measuring leads normally pass through the base

D 202 – 97 (2002)e1
FIG. 10 Electrodes for Dissipation Factor Test
plate so that a borosilicate glass bell jar or inverted desiccator 161.12 Analytical Balance.
provides the sides and top of the chamber.
161.5.2 Vacuum Pump—A vacuum pump capable of evacu- 162. Test Specimens
ating the system and maintaining a vacuum of 2.7 Pa (20 µm 162.1 The test specimens shall consist of one or more
Hg) pressure or less under continuous pumping. punched, circular layers of paper with a diameter at least 3 mm
161.5.3 Vacuum Gage. (0.12 in.) larger than that of the guarded electrode.
161.5.4 Necessary Vacuum Hardware, for example, valves,
tubing, etc. 163. Procedure
161.5.5 Flexible Tubing, especially rubber or vinyl tubing, 163.1 For papers 0.04 mm (0.0015 in.) or less in thickness,
should be used only as a means of making flexible joints stack sufficient sheets to make a pad as close as possible to 0.10
because of a tendency to leak or outgas. mm (0.004 in.) in thickness, plus two cover sheets. Remove the
161.6 Heating Equipment—Equipment to provide a means stack from between the cover sheets with tweezers and mount
of heating electrodes and specimen within the vacuum chamber on the bottom electrode. Never touch the specimen with bare
to the specified temperature(s). An infrared bulb or a set of hands.
incandescent bulbs mounted, outside of the chamber so as to 163.1.1 For papers greater than 0.04 mm and less than 0.25
provide as uniform heating of the chamber as possible, and mm (0.010 in.) in thickness, prepare a stack of one or more
surrounded by a heat reflector, have been found suitable. A specimen sheets plus outside cover sheets. Remove the speci-
heating mantle to fit the desiccator, if used, is also acceptable. men stack from between the cover sheets with tweezers and
161.7 Temperature Measurement and Control—A thermo- mount on the bottom electrode.
couple embedded in the guard plate with small diameter leads 163.1.2 Prepare specimens of at least two sheets for thick-
carried through the base plate will provide a suitable means of nesses between 0.4 and 0.25 mm in order to minimize the effect
recording the temperature, and when used with a pyrometer of irregularities of the paper-electrode interfaces which might
controller, will provide a means of controlling temperature. reduce the effective paper density between electrodes. The
electrode area should be such that the capacitance of multisheet
NOTE 28—In any specific test equipment, it is necessary to determine
experimentally the relationship between the measured temperature and the specimens of this thickness range will be within the capaci-
actual temperature of the specimen under conditions which match those of tance range of the bridge.
the dissipation factor measurement as closely as possible. Temperature 163.1.3 For papers over 0.25 mm and up to 0.75 mm (0.030
calibrations should be performed periodically and whenever changes are in.) in thickness, a single sheet is sufficient. For papers within
made in the system that might affect the relation between observed this thickness range care must be taken to eliminate or prevent
temperature and true specimen temperature. any curl of the specimen between the electrodes. Added
161.8 Punch Die—Steel circle-punching dies as required to dead-weight pressure might be required to eliminate curl.
cut specimens. A hardwood block or suitable backing support 163.1.4 For sheet materials greater than 0.75 mm in thick-
may be required to hold the paper during punching. ness, such as paperboard or pressboard, special electrode or
161.9 Air-Drying Equipment—Equipment to provide a cell construction may be required to ensure elimination of air
means of introducing thoroughly dried air into the vacuum gaps due to curl. A thin metal foil electrode set applied with a
chamber (for example, a train including sulfuric acid and minimum of silicone grease is recommended for this purpose,
phosphorus pentoxide, or activated alumina drying apparatus). such as described in Test Methods D 150. A guard electrode
161.10 Thickness-Measuring Apparatus— A dead-weight configuration can be made according to the method described
dial micrometer as specified in 19.1.1.2, unless thickness is in Test Methods D 150. Accurate concentric alignment of
measured by the air-capacitance method, or other micrometer guarded and unguarded electrodes might require an aligning
as described in Test Methods D 374. fixture, as indicated in Test Methods D 150. Hold the guarded
161.11 Sample Bottles—Bottles with ground-glass stoppers and unguarded electrode foil disks by an opposing pair of rigid
for storage and transfer of specimens. metal electrodes, plus a top dead weight. Make electrical
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D 202 – 97 (2002)e1
connections by means of the rigid electrode and dead-weight rather than to a density determined by a subsequent mechanical measure-
system. The guard electrode should be of diameter sufficient to ment.
permit attachment of a clip or soldered lead. Support the guard 163.5 Remove the specimen from the cell with tweezers. As
electrode lead so as not to cause movement of the guard quickly as possible punch a smaller diameter piece from the
electrode. specimen and place it in a stoppered weighing bottle.
163.2 Heat the specimen under continuous vacuum at a 163.6 Determine the weight of the specimen and previously
temperature not less than 105°C (for cellulose paper) for a tared bottle on an analytical balance, from which specimen
--`,,,`,`,`,`````,,,```,,`,,`,`-`-`,,`,,`,`,,`---
period of time sufficient to dry the specimen. weight can be determined.
NOTE 29—The specimen is considered dry when the dissipation factor 163.7 Remove the specimen and immediately determine the
does not decrease with increased time of drying. Usually 16 h at 115°C specimen thickness by a dead-weight dial micrometer in
and 2.7 Pa or less will suffice for cellulose papers. Completeness of drying accordance with Sections 18 to 24 for papers of thickness
can be checked by redrying and retesting the undisturbed specimen. The 0.040 mm (0.0015 in.) or less. For papers of thickness greater
two plots of dissipation factor versus temperature will be identical if the than 0.040 mm, measure the thickness in accordance with Test
specimen is completely dry. (The curves will also be identical if equal Methods D 374 by agreement between the seller and the
amounts of moisture are accidentally admitted after each drying run.) For
papers of materials other than cellulose fibers, modifications of specimen
purchaser. Thickness measurement is not required if a mea-
drying might be required. surement of thickness by air-gap electrodes has been made.
163.8 Calculate the apparent density (dry-dry basis) from
163.3 Break the vacuum with dry air and allow the speci- the weight, the known area, and the thickness of the piece cut
men to cool. Measure the dissipation factor and capacitance of in 163.5.
the specimen at intervals of approximately 10 to 20°C at a
voltage stress sufficient to provide the necessary precision, but 164. Report
not exceeding 2 kV/mm (50 V/mil) until the specimen has 164.1 Report in accordance with Section 14, and include the
cooled to 40°C or below. following information:
163.3.1 If the dissipation factor rises rapidly as the system 164.1.1 Curve of dissipation factor as a function of tem-
cools to room temperature, it is an indication that moisture is perature, or a tabulation of dissipation factor at specified
entering the system, either from leakage through a faulty seal temperatures as determined by interpolation of the dissipation
or because of inadequate drying of the air drawn into the factor-temperature curve. Extrapolation is not permitted.
system through the drying train. The cause of the moisture 164.1.2 Thickness of the specimen, the number of sheets
entry must be determined and corrected before redrying of the used, the electrode pressure applied, the applied voltage,
specimen and redetermination of the dissipation factor. A whether conforming foil electrodes were used (where appli-
positive pressure of dry air swept continuously through the cable), and the method of thickness measurement.
system and across the specimen is recommended. 164.1.3 Permittivity of the specimen at a temperature
163.4 Measure the capacitance of the supplementary airgap agreed upon between the seller and the purchaser, and calcu-
electrode where used. lated in accordance with Test Methods D 150, and
NOTE 30—A supplementary guarded electrode, as illustrated in Fig. 11, 164.1.4 Apparent density of the specimen in grams per
which has at all times the same separation from the upper electrode as that cubic centimetre.
of the main electrode, may be used to determine thickness by measure-
ment of its capacitance in dry air. The thickness, t, is calculated as follows: WATER-EXTRACTABLE CHLORIDES
t 5 ~K 3 A!/C (14)
165. Scope
where: 165.1 This test method covers the determination of water-
K = 0.885, for t, mm and A, cm2,
K = 0.2249, for t, in. and A, in.2,
extractable chlorides in electrical insulating paper.
t = separation of electrodes, 165.2 Two methods are described; a potentiometric titration
A = effective area of electrodes (see Test Methods D 150), and method, and a progressive dilution method.
C = capacitance, pF.
It is generally more accurate to measure the actual electrode separation 166. Summary of Test Methods
in this way to determine specimen density at the time of the electrical 166.1 Soluble chloride is determined by extracting with
measurement rather than by micrometer measurement of thickness. The
water under standard conditions and either titrating the dis-
dissipation factor and capicitance of the specimen are related directly to
the density of the specimen at the time of the electrical measurement
solved chloride potentiometrically (Method A), or finding the
maximum dilution at which it will produce a visible opales-
cence with silver nitrate (Method B). For routine control
applications an abbreviated extraction procedure may be used
with either test method.

167.1 The purity of papers that are used as electrical
insulation is of great importance in many applications. The
presence of chloride may adversely affect the electrical prop-
FIG. 11 Guarded Electrode for Determining Thickness erties of the paper.

D 202 – 97 (2002)e1
167.2 Method A with short time extraction is suitable as a 169.10 Tongs, stainless steel.
routine control and acceptance test for all levels of water 169.11 Medicine Dropper.
soluble chloride. Method A with long term extraction is
suitable for both routine and referee testing for water-soluble 170. Reagents
chloride at all concentrations. Method B with either long time 170.1 Water, conforming to Type III of Specification
or short time extraction is restricted to use for water soluble D 1193, and free of chlorides as detected by this test method.
chloride levels of 16 ppm (parts per million) or greater and 170.2 Acetone, chloride-free, reagent grade. If a blank
where the within-range method of reporting is acceptable. titration shows the presence of chloride, reflux 1 L of the
acetone with 0.1 g silver nitrate for 30 min. Distill the acetone
168. Interferences from the silver nitrate, discarding the first 25 mL to flush the
168.1 The presence of water soluble halide ions other than apparatus and receiver. Distill approximately 90 % of the
chloride will be detected by these test methods, as will the acetone and discard the remaining liquid. The chloride ion
presence of any substance that forms an insoluble silver concentration of the acetone should be equivalent to less than
compound or otherwise interferes with the response of silver to 0.01 mL of 0.0025 N AgNO 3 solution per 100 mL of the
the silver electrode in Method A. acetone.
168.2 The amount of chloride ions measured when the test 170.3 Nitric Acid (1 %)—Add 1 mL of concentrated nitric
is applied to electrical insulating paper of good quality is very acid (sp gr 1.42) to 80 to 90 mL of water. Then dilute with
small, from a fraction of a part per million to a few parts per water to 100 mL.
million. For this reason, extreme care must be taken in all 170.4 Silver Nitrate, Standard Solution (0.0025 N):
phases of testing, from sampling to final addition of reagents. 170.4.1 Dry the silver nitrate overnight in a desiccator
The specimen should not be touched with the hands. All before preparing the solution. Protect both the solid AgNO3
glassware, apparatus, and the atmosphere in contact with the and the solution from light by storage in brown glassware in a
sample or its extract solution must be free of contamination, dark room or cabinet.
such as chemical vapors, tobacco smoke, etc. The test method 170.4.2 Weigh 424.7 6 0.1 mg of reagent grade silver
requires titration of a simultaneous blank. The level of chloride nitrate. Transfer it quantitatively to a 1-L volumetric flask and
indicated by the blank will indicate the amount of interfering add sufficient water to dissolve the AgNO3. Add 3 mL of
contamination of the analysis. concentrated HNO 3 (sp gr 1.42), mix, then add water to the 1
L mark of the volumetric flask. Water and flask should be as
Method A close as possible to the standard volumetric temperature
indicated on the flask. Standardize against a known chloride
169. Apparatus standard. Check the titer at least monthly.
169.1 Electrometric Titrimeter20—A high-impedance milli-
voltmeter having a scale with the smallest ruled interval not 171. Sampling
greater than 5 mV and an ultimate sensitivity of 0.5 mV or less. 171.1 Sample in accordance with Sections 5 to 13. Take a
169.2 Standard Glass Electrode.21 minimum of 12 g per test unit.
169.2.1 Although the glass electrode is preferred, a mercu-
rous sulfate reference electrode may be used. 172. Preparation of Apparatus
169.3 Microburet, 1.0 mL capacity graduated in 0.01 mL 172.1 Clean all glassware with sulfuric acid-dichromate
divisions. solution, rinse thoroughly with reagent water, and reflux the
169.4 Magnetic Stirrer, with glass-covered or PTFE- glassware extraction assembly for a few minutes with reagent
fluorocarbon-coated stirring bar. water. Steam other glassware with boiling reagent water.
169.5 Hot Plate. Following cleaning and rinsing, take great care not to handle
169.6 Tall-form Beaker. the glassware directly with the hands or otherwise expose it to
169.7 Extraction Glassware. potential contamination. Polish the silver billet electrode with
169.7.1 Erlenmeyer Flasks, 300 mL, standard taper 24/40 No. 4/0 emery paper at least once each day or on dull
joint. appearance. Between tests, clean the electrodes by rinsing with
169.7.2 Condenser, water-cooled, standard taper 24/40 water and acetone.
joint.
169.7.3 Fluorocarbon Sleeve, standard taper 24/40. These 173. Procedure
sleeves eliminate the need for grease, which is a possible 173.1 Extraction:
contaminant. 173.1.1 Cut the specimen into approximately 6-mm squares
169.8 Balance, with 0.01 g accuracy. with clean scissors.
169.9 Buchner Funnel, coarse-fritted glass. 173.1.2 Weigh 4.00 6 0.01 g of the specimen and introduce
it into a 300-mL Erlenmeyer flask without allowing the
specimen to contact any contaminating surface.
20
The Radiometer P501, and Leeds & Northrup standard 1199-62 have been 173.1.3 Add 100.0 6 0.1 g of water to the flask.
found satisfactory for this purpose.
21
Radiometer K-601, Beckman No. 40455 mercury sulfate sleeve electrode with
173.1.4 Attach the condenser to the flask and reflux vigor-
Beckman No. 8548 saturated potassium sulfate filling solution has been found ously for 60 min (referee method) or for 10 min (routine
satisfactory for this purpose. method).
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D 202 – 97 (2002)e1
173.1.5 Determine the moisture content of the sample on 95 % probability limits, expressed as a percentage of the grand
another portion. Weigh this specimen simultaneously with the average, are as follows, for the referee method only:
test specimen. 95 % Probability Limits of Results Expressed as
Level of
173.1.6 Remove the apparatus from the hot plate, cover the Percentage of Grand Average
Grand Average
top of the condenser tightly with a piece of aluminum foil, and Water-Soluble
Number of Tests per Laboratory
Chloride, ppm
allow the entire assembly to cool to room temperature. Cooling 2 3 4 5 10
may be facilitated by careful immersion of the flask in a 1 100 80 70 60 40
7 30 30 20 20 15
container of cold water. 40 10 10 8 8 5
173.2 Titration:
173.2.1 Filter or decant the cooled extract solution and 176.2 This test method has no bias because the value for
weigh 25.0 6 0.1 g into a tall-form beaker. Add 125 mL of chlorides is defined in terms of the test method.
acetone, then 15 drops of 1 % HNO3.
Method B
173.2.2 Place a stirring bar into the beaker, then place the
--`,,,`,`,`,`````,,,```,,`,,`,`-`-`,,`,,`,`,,`---
beaker on the magnetic stirrer and adjust the stirrer speed so 177. Apparatus
that the surface of the liquid is not broken.
173.2.3 Immerse the electrodes into the liquid. When the 177.1 Apparatus in accordance with 169.4 through 169.9,
meter is stable, changing less than 3 mV/min, take an initial except substitute 500-mL Erlenmeyer flasks.
reading and start the titration. 177.2 Test Tubes, heat-resistant glass, 25 mm in diameter by
173.2.4 Add the standard AgNO3 solution in 0.01-mL 100 mm in length.
increments and record the change in millivolts. Normally, 177.3 Comparator, see Fig. 12.
small total amounts of solution are required for the titration,
178. Reagents
thus the use of small increments of titrant. Allow sufficient time
between additions to establish a steady and equilibrium emf 178.1 Nitric Acid, concentrated reagent, sp gr 1.42.
reading. If three or four 0.01-mL additions result in less than 1 178.2 Silver Nitrate Solution (50 g/L)—Dissolve 50 g
mV/0.01 mL change, slightly larger amounts may be added reagent grade silver nitrate in 1 L of water.
until such change is observed. Addition of titrant should then
be reduced to 0.01 mL per addition for completion of the 179. Procedure
titration. The end point is the point on the titration curve of 179.1 Prepare the specimen in accordance with 173.1.1.
millivolt versus millilitre of titrant at which the greatest change Weigh 5.00 6 0.01 g into a 500-mL Erlenmeyer flask.
of emf per unit volume of titrant is found. Determine and Determine moisture content in accordance with 173.1.5.
record the volume of titrant required to reach the endpoint. 179.2 Add 200.0 6 0.2 g of water. Attach the condenser and
reflux as in 193.1.4, according to short-time or long-time
NOTE 31—Duplicate titrations on a single extract should agree to 60.01
mL. Duplicate specimens from the same sample should agree to within 6
extraction desired.
5 %, except at low chloride levels where percentage differences may be 179.3 Filter or decant the extract and fill two test tubes
greater. Greater differences indicate errors in procedure. within 6 mm of the top.
179.4 Add 2 drops of HNO3 to each tube.
173.2.5 Titrate a reagent blank consisting of 25 g of water,
179.5 Place the tubes in the comparator and add 3 drops of
125 mL acetone, and 15 drops of 1 % HNO3.
AgNO3 solution to one tube. Let stand for 5 min, then compare
174. Calculation to detect turbidity using the comparator.
174.1 Calculate the chloride content of the specimen as 179.6 If the tube containing the AgNO3 solution shows no
follows: turbidity, the water soluble chloride content of the specimen is
less than 4 ppm.
~A 2 B!N 3 35.46 179.7 If the tube shows turbidity, dilute another portion of
Chloride, ppm 5 D/4 3 10 3 (15)
the extract with an exactly equal volume of water and repeat
where: 179.4 through 179.6.
A = 0.0025 N AgNO3 solution for specimen end point, 179.8 Repeat 179.7, with progressive 1-to-1 dilutions, until
mL, turbidity does not appear.
B = 0.0025 N AgNO3 solution for blank end point, mL, 179.9 The water and reagents, when mixed in the amounts
N = normality of the AgNO3 solution, and and proportions of the test, must show a clear blank. A prepared
D = weight of specimen, oven-dry basis, g. NaCl solution of 0.1 ppm Cl− must also show a clear blank test.
175. Report 180. Calculation

175.1 Report in accordance with Section 14, except report 180.1 Chloride content in parts per million when turbidity is
chlorides in ppm to the next higher integer above the value last detected is more than
found. 4 3 ~1/dilution used in test! (16)
176. Precision and Bias 180.2 Chloride content in parts per million for no turbidity
176.1 In between laboratory testing where each laboratory is less than
makes a given number of tests and reports the average, the 4 3 ~1/dilution used in test! (17)

--`,,,`,`,`,`````,,,```,,`,,`,`-`-`,,`,,`,`,,`---
D 202 – 97 (2002)e1
FIG. 12 Light Comparator
Example: A test showed perceptible turbidity after three 184. Summary of Test Method
dilutions but none after a fourth. Chloride is therefore more 184.1 Electrical insulating paper is immersed in a solution
than of potassium ferricyanide (K3Fe(CN)6) solution. The potas-
4 3 1/~1/2 3 1/2 3 1/2! 5 2 2 3 2 3 5 2 5 (18) sium ferricyanide forms Turnbull blue with iron as follows:
and less than 3 Fe11 1 2 Fe~CN!6 → Fe3~Fe~CN!6!2↓ (20)
2 4
4 3 1/~1/2 3 1/2 3 1/2 3 1/2! 5 2 3 2 5 2 6
(19) The paper is then removed from the solution and placed over
an inspection light. Blue spots sufficiently large to indicate the
181. Report presence of iron particles are then counted and reported.
181.1 Report in accordance with Section 14.
181.1.1 Report chloride content as a range, perceptible to
not perceptible. In the above example, the reported value 185.1 The purity of electrical insulating paper is of extreme
would be 2 5 to 26 (32 to 64) ppm chloride. importance in most applications and the presence of particles
of metal would adversely affect the insulating properties of the
182. Precision and Bias paper.
182.1 The reproducibility of this test has not been demon- 186. Apparatus
strated to be sufficiently accurate below 24 ppm for acceptance
as a standard test. Above this level, there should be no 186.1 Inspection Light.22
disagreement as to the range when one-to-one dilutions are 186.2 Soaking Tray, glass, with a cover.
used. 187. Reagents
182.2 This test method has no bias because the value for
187.1 Agar.
chlorides is defined in terms of the test method.
187.2 Potassium Ferricyanide (K3Fe(CN)6).
PARTICULATE IRON 187.3 Sodium Chloride (NaCl).
187.4 Test Solution—Dissolve 9.75 g of NaCl, 9.75 g of
183. Scope K3Fe(CN)6 and 0.975 g of agar in water and make up to 1 L.
183.1 This test method covers the determination of the After mixing, it may be stored in a glass bottle until used.
presence or absence of iron particles in electrical insulating
paper up to 0.050 mm (0.002 in.) thick. This test method may 22 2
I R’s Glow Box, Model 12-20E-3, manufactured by Instruments for Research
be useful for papers over 0.050 mm in thickness, but may and Industry, Cheltenham, PA 19100, has been found satisfactory for this test
require a modification in the detection technique. method.

D 202 – 97 (2002)e1
188. Test Specimen tightly sealed bottle, and solution should be prepared from the reagent
periodically and tested for activity with a known source of particulate
188.1 Take a test specimen 250 by 300 mm (10 by 12 in.) or copper.
of equivalent area from the sample obtained in accordance with
Sections 5 to 13. 196.4 Water.
197. Test Solution
189. Procedure
197.1 Mix the following reagents in the order given, agitat-
189.1 Completely immerse the specimen in the ferricyanide
ing the solution (Note 32) after each addition until the solution
solution, but avoid contact of the paper with the bottom of the
is homogeneous:
tray.
Water 500 mL
189.2 After 5 6 0.2 min remove the specimen and place it Ammonium hydroxide 43 mL
over the inspection light. Nitric acid 9 mL
189.3 With the light on, examine the specimen for blue Sodium diethyldithiocarbamate 2.9 g
spots (Turnbulls blue) of 0.06 mm2 or larger. 198. Test Specimens
189.4 The presence of blue spots 0.06 mm2 or larger is
evidence of the presence of particulate iron. 198.1 See 188.1.
189.5 Discard the solution in the try after 8 h, or when it 199. Procedure
acquires a bluish tinge, whichever occurs first.
199.1 Completely immerse the specimen in the carbamate
190. Report test solution, but avoid contact of the paper with the bottom of
the tray.
190.1 Report the presence or absence of particulate iron in 199.2 After 10 6 0.2 min in the test solution, remove the
accordance with Section 14. specimen and place it over the inspection light.
191. Precision and Bias 199.3 Under illumination examine the specimen for brown
spots 0.06 mm2 or larger.
191.1 No information is presented about either the precision 199.4 The presence of brown spots 0.06 mm2 or larger is
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or bias of this test method because the test result is nonquan- evidence of the presence of particulate copper.
titative.
200. Report
PARTICULATE COPPER
200.1 Report the presence or absence of particulate copper
192. Scope in accordance with Section 14.
192.1 This test method covers the determination of the 201. Precision and Bias
presence or absence of copper particles in electrical insulation 201.1 No information is presented about either the precision
paper up to 0.050 mm (0.002 in.) in thickness. Suitability of the or bias of this test method because the test result is nonquan-
test method for use with thicker papers has not been estab- titative.
lished.
SILVER TARNISHING BY PAPER
202. Scope
193.1 Electrical insulating paper is immersed in sheet form
in a solution of sodium diethyldithiocarbamate. The test 202.1 This test method covers the detection of the presence
solution reacts with any copper particles present to form brown in papers of those contaminating compounds that will react in
spots. The paper is then removed from the solution and placed the presence of heat and moisture to tarnish or stain silver.
over an inspection light. Brown spots due to copper particles 203. Significance and Use
are determined and reported.
203.1 The most common reactive contaminants which will
194. Significance and Use tarnish silver are compounds of sulfur. Many reactive sulfur
compounds cause progressive deterioration of the insulation
194.1 See 185.1.
resistance and loss characteristics of dielectric systems. Also,
195. Apparatus sulfides tend to react with the conductive metals in electrical
apparatus and can severely reduce the efficiency of contact
195.1 See 186.1 and 186.2.
areas.
196. Reagents 203.2 Insufficiently-washed kraft pulps and sulfur-
containing lubricants on tools used to cut insulating shapes are
196.1 Ammonium Hydroxide (sp gr 0.90)—Concentrated among the sources of reactive sulfur in electrical insulating
ammonium hydroxide (NH4OH). papers and boards.
196.2 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
(HNO3). 204. Procedure
196.3 Sodium Diethyldithiocarbamate. 204.1 From the sample obtained in accordance with Sec-
NOTE 32—Both the sodium diethyldithiocarbamate reagent and its tions 6 through 13 take specimens and test them in accordance
solution are subject to deterioration. The reagent should be stored in a with TAPPI T-444.

D 202 – 97 (2002)e1
205. Report ing; conducting paths; density; dielectric strength; dimensions;
205.1 Report in accordance with Section 14 and TAPPI dissipation factor; edge-tearing resistance; fiber analysis; fold-
T-444. ing endurance; grammage; heat stability; impregnation time;
internal-tearing resistance; moisture content; paper; paper-
206. Keywords board; particulate copper; particulate iron; permittivity; pH;
206.1 absorption; acidity; air resistance; alkalinity; aqueous roll dimensions; sampling; sheet dimensions; silver tarnishing;
extract conductivity; aqeous extract pH; ash content; basis solvent-soluble content; specific gravity; surface friction; ten-
weight; board; bursting strength; chloride content; condition- sile properties; tearing resistance; thickness
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An American National Standard

Designation: D 202 – 97 (2002)e1

Standard Test Methods for

e1 NOTE—Editorial changes made to footnotes 13-15, and Section 1 September 2002.

1. Scope thetic, organic, or inorganic; and flexible polymeric binder

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material that can be extracted from a dry specimen by a

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Property Minimum Number Minimum Number

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NOTE 6—When measuring the thickness of noticeably compressible

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42. Significance and Use

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52. Calculation W = mass of paper specimen, g.

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of the flask when the siphon cup is full.

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FIG. 6 Sliding Block for Surface Friction Test

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118. Calculation 120.1.2 In each case, the coefficient of variation of a test

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138. Scope 142. Test Specimen

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157. Report 161. Apparatus

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FIG. 10 Electrodes for Dissipation Factor Test

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167. Significance and Use

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175. Report 180. Calculation

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FIG. 12 Light Comparator

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