ASTM D29-98

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D29–98
Standard Test Methods for
Sampling and Testing Lac Resins
ThisstandardisissuedunderthefixeddesignationD 29;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginal
adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscript
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.
1. Scope (Gardner Color Scale)
D 1545 Test Method for Viscosity of Transparent Liquids
1.1 These test methods cover procedures for sampling and
by Bubble Time Method
testing orange shellac, button lac, garnet lac, and bleached lac.
D 1959 Test Method for Iodine Value of Drying Oils and
1.2 The sampling procedures and test methods appear in the
Fatty Acids
following order:
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
Sections
poses
Sampling:
Orange Shellac, Button Lac, and Garnet Lac 3
Bleached Lac 4
SAMPLING
Identification of Samples 5
General Requirements for Test Methods:
3. Orange Shellac, Button Lac, and Garnet Lac
Reagents 6
Source and Preparation of Portions of Sample for
3.1 Lot Size—For the purpose of sampling, the quantity of a
Tests 7
lot of any one of these types of lac resin shall not exceed 500
Insoluble Matter 8 to 9.5
Iodine Value 10 to 10.3 bags or packages. The net weight of lac resin in each bag or
Purity 11 to 13.2
package shall not exceed 75 kg.
Volatile Matter (Moisture) 14 to 15.2
3.2 Source and Number of Samples—Only original un-
Wax 16to16.4
Matter Soluble in Water 17 to 17.2
opened bags or packages shall be sampled. Ten percent of the
Ash 18 to 18.2
containersineverylotoflacresinshallbetakenatrandom,but
Color 19 to 19.4.3
not less than 5 nor more than 25 containers shall be taken.
Color of Orange Shellac 20 to 20.4.4
Acid Value 21 to 21.4
3.3 Free-Flowing Lac Resins—In sampling free-flowing lac
Orpiment 22 to 22.4
resins, samples shall be drawn from different places in each
Saponification Value 23 to 23.4
container in double handfuls or by means of a suitable sampler
1.3 This standard does not purport to address all of the
such as a grain sampler. A total of approximately 2.7 kg shall
safety concerns, if any, associated with its use. It is the
be taken.
responsibility of the user of this standard to establish appro-
3.4 Blocked or Matted Lac Resin—Pieces of blocked or
priate safety and health practices and determine the applica-
matted lac resin shall be chipped with an axe, pick, or other
bility of regulatory limitations prior to use. Specific hazard
suitable instrument from each container taken for sampling.
statements are given in Note 1.
Approximately the same amount shall be taken from each
container and the total amount taken shall be about 2.7 kg. The
2. Referenced Documents
pieces of lac resin shall then be ground to pass a No. 4
2.1 ASTM Standards:
(4.75-mm) sieve. All sieves referenced must conform to the
D 304 Specification for n-Butyl Alcohol (Butanol)
requirements of Specification E 11 .
D 331 Specification for 2-Ethoxyethanol
3.5 Preparation of Samples for Observation or Analysis—
D 1193 Specification for Reagent Water
Whether free-flowing or rough ground, as in the case of
D 1544 Test Method for Color of Transparent Liquids
blocked lac resin, the entire sample representing any lot shall
be thoroughly mixed and divided into halves. The use of a
mechanical mixer is recommended for mixing the resin and a
1 riffle sampler for dividing it into quarters. When these devices
ThesetestmethodsareunderthejurisdictionofASTMCommitteeD-1onPaint
are not available for use, the entire sample shall be mixed,
and Related Coatings, Materials, and Applications and are the direct responsibility
of Subcommittee D 01.33 on Polymers and Resins.
Current edition approved June 10, 1998. Published October 1998. Originally
{1
published as D 29 – 14 T. Last previous edition D 29 – 81(l993) .
2 4
Annual Book of ASTM Standards, Vol 06.04. Annual Book of ASTM Standards, Vol 06.01.
3 5
Annual Book of ASTM Standards, Vol 11.01. Annual Book of ASTM Standards, Vol 06.03.
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D29–98
heaped, and quartered along two diameters that intersect at 5. Identification of Samples
right angles and the opposite quarters combined. One half the
5.1 The following information shall be legibly placed on the
sample, thus obtained, shall then be mixed and divided into
label, which shall be securely attached to each sample con-
quarters as before. Each quarter shall be placed in an airtight
tainer: date of the sampling, number of bags, barrels or
container, sealed, labeled (Section 5), and sent to the interested
packages sampled, total number of containers in the lot,
parties as the “original observation sample.” When agreed
condition of the containers and their contents, manufacturer’s
upon between the seller and the purchaser, the “original
name, lot and code numbers of the containers, and the purpose
observation sample” shall be used for the determination of
identification, namely “original observation sample” or
volatile matter (moisture) (Sections 14 to 15, as applicable).
“sample for determination of volatile matter (moisture)”,
The other half of the sample shall be ground to pass a No. 10
“reserve sample” or “prepared sample” as may apply.
(2.00-mm)sieve,mixedthoroughly,anddividedintotwoequal
portions A and B. Portion A shall be labeled the “reserve TEST METHODS
sample.” Portion B shall then be ground to pass a No. 25
6. Reagents
(710-µm) sieve, mixed thoroughly, and quartered as described
above. Each quarter shall be packaged in an airtight container, 6.1 Purity of Reagents—Reagent grade chemicals shall be
sealed, labeled “prepared sample,” and sent to the testing
used in all tests. Unless otherwise indicated, it is intended that
laboratory for analysis. allreagentsshallconformtotheSpecificationsoftheAmerican
Chemical Society, where such specifications are available.
4. Bleached Lac Other grades may be used, provided it is first ascertained that
the reagent is of sufficiently high purity to permit its use
4.1 Lot Size—For the purpose of sampling, the quantity of a
without lessening the accuracy of the determination.
lot shall not exceed 200 packages.
6.2 Purity of Water—Unless otherwise indicated, references
4.2 Source and Number of Samples—Only original un-
to water shall be understood to mean reagent water conforming
opened packages shall be sampled. Twenty percent of the
to Type II of Specification D 1193.
containers in every lot shall be taken at random, but not less
than two containers in any lot shall be taken, except in the case
7. Source and Preparation of Specimens for Tests
where the entire lot is packaged in a single container.
7.1 Each portion of sample for use in a given test shall be
4.3 Dry Bleached Lac (Free-Flowing)—Samples shall be
taken from the sample of lac resin only after it has been mixed,
drawn with a scoop or suitable sampler from different parts of
either by rolling on paper or by rolling and tumbling in its
each container directly after the packages are opened or bored.
airtight container, as the condition of the sample requires, a
Approximately 450 g shall be drawn from each container. The
sufficientnumberoftimestoensureuniformityofthespecimen
samples shall be combined, mixed thoroughly, and where
taken. The test specimens shall be taken from the“ prepared
larger than 1.4 kg, shall be reduced by quartering as prescribed
sample”(3.5or4.6),asreceived,exceptinthefollowingcases:
in 3.5 to a sample of this size.
7.1.1 When it has been previously agreed upon between the
4.4 Dry Bleached Lac (Blocked or Matted)—Samples ag-
seller and the purchaser that the “original observation sample”
gregating at least 450 g shall be chopped or chiseled from
shall be used for the determination of volatile matter (mois-
different parts of each container. The composite sample from
ture). In this case, the “original observation sample” shall be
all the containers shall be quickly crushed to lumps about 25
mixed, quartered, ground, and sieved in accordance with the
mm square or smaller. The crushed lac resin shall be well
procedure described in 3.5 for obtaining the “prepared
mixed and where the amount is larger than 1.4 kg, it shall be
sample.” All operations shall be done as expeditiously as
reduced by quartering, as prescribed in 3.5, to a sample of
possible and the test specimen taken immediately after the
approximately this size.
sieved sample has been thoroughly mixed, to avoid any
4.5 Hanks, Bars, or Crushed Free-Ground Bleached Lac—
possible loss by evaporation.
This material, which generally contains approximately 25 %
7.1.2 When the “prepared sample” is known to have a high
moisture, shall be sampled by the procedures described in 4.3
moisturecontent,asinthecaseofcertainformsofbleachedlac
or 4.4, as applicable.
(4.5), it shall be dried to a moisture content of 6 % before the
4.6 Preparation of Samples for Analysis—The composite
testspecimensaretaken.Thelacresinshallbedriedbyplacing
sample obtained as described in 4.3 or 4.4 shall be mixed
it in a thin layer in a flat-bottom dish (loosely covered to
thoroughly and divided into two equal portions A and B as
prevent dust contamination) and exposing it to the atmosphere
prescribed in 3.5. Each portion shall be placed in a clean, dry
at room temperature for 24 h and then desiccating it over
glass jar provided with a rubber-sealed cap or an airtight
anhydrous calcium chloride. The partially dried lac resin shall
friction-top tin can. Portion A shall be labeled “reserve
be kept in a clean, dry, airtight container, and shall be
sample.” Portion B obtained in accordance with 4.3 or 4.4 shall
be further ground to pass a No. 20 (850-µm) sieve, thoroughly
mixed and replaced in the jar, sealed and labeled “prepared
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
sample.” Portion B obtained in accordance with 4.5 shall be
listed by the American Chemical Society, see Analar Standards for Laboratory
further ground to pass a No. 10 (2.00-mm) sieve, thoroughly
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
mixed, replaced in the jar, sealed, labeled “prepared sample,”
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
and sent to the laboratory for analysis. MD.
D29–98
thoroughly mixed by rolling and tumbling in the container
before the specimens are taken for analysis.
INSOLUBLE MATTER
8. Test Method A—For Orange Shellac, Button Lac,
Garnet Lac, and Regular Bleached
8.1 Apparatus:
8.1.1 Condenser—A four-bulb Allihn condenser of the di-
FIG. 2 Hot-Water Bath for Insoluble Matter,
mensions and design shown in Fig. 1.
Test Method A
8.1.2 Siphon Tube—A Knoefler siphon tube of the dimen-
sions shown in Fig. 1.
8.1.3 Filter Tube—A carbon filter tube of the dimensions
NOTE 1—Precaution: The reagents and samples used in these methods
shown in Fig. 1.
may, under some conditions, be hazardous. Refer to the supplier’s
8.1.4 Flask—Aborosilicate glass Erlenmeyer flask 176 6 3 Material Safety Data Sheet for specific handling and safety precautions.
Safe laboratory handling procedures and all applicable OSHAregulations
mm in height and 48 6 1.5 mm in inside diameter at the top.
are to be followed.
8.1.5 Flask Support—A suitable ring support with an iron
clamp and a Nichrome or iron wire gauze square without an 8.3 Preparation of Extraction Thimble:
asbestos center. 8.3.1 Pass the stem of the condenser through a hole cut in
8.1.6 Extraction Thimble—Extraction thimble 26 61mm the center of a cork stopper of such size that it will tightly fit
in diameter and 60 6 1 mm in height. the flask.Adjust the cork on the stem so that the bottom of the
cork is just above the holes in the stem. Place an extraction
8.1.7 Water Bath—Ametal container with cover of the size
and design shown in Fig. 2. The container and cover shall be thimble (use new thimbles only) in the siphon tube. Suspend
the siphon tube from the stem of the condenser by passing a
made of 26-oz copper sheet. The cover shall have a flanged
hole 57 6 1 mm in diameter for a 200-mL beaker and also a piece of copper wire through the holes in the stem and
fastening the ends of the wire through the holes in the siphon
hole 35 6 1 mm in diameter for the carbon filter tube. Directly
belowthisholeinthebottomofthecontainershallbeaflanged tube. The wire shall be sufficiently long to leave about 6-mm
space between the tip of the condenser and the top of the
hole 25 6 1 mm in diameter.
8.1.8 Heating Device—An electric hot plate or bunsen siphon tube.
burner equipped with a draft shield. 8.3.2 Place 125 mL of ethyl alcohol in the flask and attach
8.1.9 Weighing Bottle—A glass-stoppered weighing bottle the flask to the condenser by means of the cork stopper. Place
of the dimensions shown in Fig. 1. theflaskonanelectrichotplateoraflasksupport.Runasteady
8.2 Solvent—Specially denatured 95 % (190 proof) ethyl streamofcoldwaterthroughthecondenser.Adjusttheflameof
alcoholconformingtoFormulaNo.1orNo.3AoftheAlcohol, the burner or the hot plate setting so as to give a cycle of filling
Tobacco and Firearms Division of Internal Revenue Service, and emptying of the siphon tube every 2 min, and extract the
U.S. Treasury Department. thimble for 30 min. Remove the extraction thimble from the
siphon tube and allow to drain and air-dry for several minutes.
8.3.3 Place the thimble in a weighing bottle and dry in an
oven for2hat105 6 2°C. Remove and stopper the weighing
bottle and cool in a desiccator. Weigh the bottle and thimble
lifting the stopper momentarily before weighing. Continue
drying and weighing as before after each hour of drying until
the loss in weight between successive weighings does not
exceed 2 mg.
8.3.4 A number of thimbles may be extracted and kept in
weighing bottles or a desiccator until needed.
8.4 Procedure:
8.4.1 Weighto1mg5 60.2gofthemixedsample(Section
7)andplaceina200-mLtall-formbeaker.Add125mLofethyl
alcohol to the beaker and place it in the hot-water bath (Fig. 2),
which has been previously heated to not less than 90°C.
Maintain the bath at this temperature, or above, during the
solution and filtration of the sample. Boil the solution for 30
min, keeping the volume of alcohol constant to ensure com-
plete solution of the lac resin.
8.4.2 Placeanextracted,weighedextractionthimble(8.3)in
the carbon filter tube (Fig. 2). Wet the thimble with hot alcohol
and decant the bo
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