NOTICE: This standard has either been superceded and replaced by a new version or discontinued.

Contact ASTM International (www.astm.org) for the latest information.

Designation: D 1417 – 03

Standard Test Methods for

Rubber Latices—Synthetic1
This standard is issued under the fixed designation D 1417; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope TABLE 1 Drying Time for Determination of Total Solids in Latex

(Drying Aid, 1 cm3 of distilled water.)
1.1 These test methods cover test procedures for synthetic
Type of Latex Drying Time, min
rubber latices ABR, BR, CR, IIR, IR, NBR, NCR, NIR, PBR,
PSBR, SBR, SCR, SIR, synthetic rubber latices having substi- SBR 2000 45
SBR 2001 45
tute carboxylic acid (COOH) groups on the polymer chain (X), SBR 2002 45
and synthetic rubber latices that are reinforced (Y). Exceptions SBR 2003 45
BR 2004 45
to the above are noted in the individual test procedures. The SBR 2005 45
test methods include procedures for sampling, and for deter- SBR 2006 45
mining total solids, volatile unsaturates (residual styrene), pH SBR 2076 45
SBR 2100 60
value, surface tension, viscosity, coagulum, bound styrene, SBR 2101 and X765 45
Mooney viscosity, mechanical stability, polystyrene reinforce- SBR 2102 60
ment in contained polymer, and residual acrylonitrile content. SBR 2103 60
BR 2104 45
NOTE 1—The nomenclature used in these test methods is in accordance SBR 2105 45
with Practice D 1418. SBR 2106 45
SBR 2107 45
1.2 The values stated in SI units are to be regarded as SBR 2108 45
standard. SBR 2109 45
SBR 2110 45
1.3 This standard does not purport to address all of the SBR 2111 45
safety concerns, if any, associated with its use. It is the SBR 2112 45
responsibility of the user of this standard to establish appro- SBR 2113 45
SBR 2114 45
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Table 1
2. Referenced Documents Procedures for Mixing Standard Compounds and Prepar-
2.1 ASTM Standards: ing Standard Vulcanized Sheets2
D 1076 Specification for Rubber—Concentrated, Ammonia D 3314 Test Method for Rubber—Chemical Analysis for
Preserved, Creamed, and Centrifuged Natural Latex2 Polystyrene Blocks in SBR (Styrene-Butadiene Rubber)
D 1331 Test Methods for Surface and Interfacial Tension of and Styrene-Reinforced Latices2
Solutions of Surface-Active Agents3 D 4483 Practice for Determining Precision for Test Method
D 1416 Test Methods for Rubber from Synthetic Sources— Standards in the Rubber and Carbon Black Industries2
Chemical Analysis2 E 70 Test Method for pH of Aqueous Solutions with the
D 1418 Practice for Rubber and Rubber Latices— Glass Electrode4
Nomenclature2 E 200 Practice for Preparation, Standardization, and Stor-
D 1646 Test Methods for Rubber—Viscosity, Stress Relax- age of Standard and Reagent Solutions for Chemical
ation, and Pre-Vulcanization Characteristics (Mooney Vis- Analysis4
cometer)2
D 3182 Practice for Rubber—Materials, Equipment, and 3. Sampling
3.1 Rubber latex tends to cream on standing. Once stratifi-
cation has occurred, the latex must be thoroughly agitated to
1
obtain a homogeneous blend as a representative sub-sample.
These test methods are under the jurisdiction of ASTM Committee D11 on
Rubber and are the direct responsibility of Subcommittee D11.23 on Synthetic The procedure required differs with the type of container and
Rubbers. facilities available.
Current edition approved June 10, 2003. Published June 2003. Originally
approved in 1956. Last previous edition approved in 1997 as D 1417 – 97.
2
Annual Book of ASTM Standards, Vol 09.01.
3 4
Annual Book of ASTM Standards, Vol 15.04. Annual Book of ASTM Standards, Vol 15.05.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 1417 – 03
3.2 Sub-Sampling from Tank Cars: 4.1.1 Tared, covered, all-metal ointment boxes, having a
3.2.1 If stratification has occurred, take separate samples capacity of approximately 50 to 60 cm3, a minimum diameter
about 75 mm (3 in.) from the top surface and about 75 mm of 38 mm (1.5 in.), and a maximum height of 23 mm (0.9 in.).
from the bottom of the tank. If results from the top and bottom The disposable aluminum liner for the metal ointment box may
samples do not agree within 1 % total solids, the contents of the be used.
car shall be thoroughly agitated until samples obtained do 4.2 Procedure:
agree within this tolerance. 4.2.1 Method A—Accurately weigh a clean, dry aluminum
foil dish. Record the weight. Measure 2 mL of sample and put
3.3 Sub-Sampling from Drums: in the aluminum foil dish. Reweigh the dish and record the
3.3.1 Blending—The latex shall be blended by one of the weight. Put the aluminum foil dish in a 170°C oven; heat for 15
following test methods: min. Remove the aluminum foil dish from the oven and let cool
3.3.1.1 Test Method A—If the drum is fitted with a bung and in a desiccator. Reweigh the aluminum foil dish. Record the
contains at least 2 % air space, lay it on its side and roll back weight. Calculations: A = weight of dish empty; B = weight of
and forth briskly for not less than 10 min. Then turn the drum dish + sample; C = weight of dish + residue;
upside down for about 15 min and repeat the rolling operation ~C – A!~100!
for an additional 10 min. If the drum contains less than 2 % air ~B – A! 5 % Total Solids (1)

space, transfer the contents to a larger vessel and thoroughly Report the total solids to the nearest 0.1 %.
stir, preferably by means of a perforated steel disk plunger. 4.2.2 Method B—The percent solids is determined by mea-
Stirring for about 10 min will normally suffice. If the drum is suring gravimetrically the solids remaining after volatilizing
of the open-head type, remove the end head and thoroughly stir off the liquid portion.
the contents, preferably by means of a perforated steel disk 4.2.2.1 Instrument Conditions—The following instrument
plunger. Stirring for about 10 min will normally suffice. conditions are based on work done with a Denver IR-100:
3.3.1.2 Test Method B—Agitate the contents of the drum by Oven Temperature—145°C
Slope—0.05 %/min
means of a suitable motor-driven stirrer for as long as is Program—No. 1
necessary to disperse the cream. Excessive stirring and unnec- A1 pans—Fisher #01-913-356
essary exposure of the latex to air must be avoided. A suitable Fiber paper—Fisher #01-913-318

type of stirrer consists of a collapsible two-bladed stainless Place a glass fiber filter circle on an aluminum pan. Open the
steel propeller of 11 cm minimum diameter, when fully lid of the IR-100 and center the pan (with filter) between the
opened, mounted on a stainless steel shaft sufficiently long for four prongs of the“ X”-shaped holder. Close the lid and press
the propeller to be distant about one quarter the height of the the START button. When display reads “tare pan,” press the
latex from the bottom of the drum. The stirrer shall be operated TARE button. Raise the lid and place about 3.0 g of latex in a
at a minimum speed of 900 r/min. If desired, two propellers circle on the filter paper. Again close the lid. Wait 10 seconds,
may be used on the same shaft, the lower one being near the then press the START button. The instrument will automati-
end of the shaft. The shaft speed shall give a brisk turnover cally run for about 4 min then shut off. Read the percent (%)
without creating a vortex. The part of the equipment immersed solids directly from the printout paper or from the display
in the latex must contain no copper or brass. screen. Report the value to the nearest 0.1 %.
3.3.2 Removal of Sub-Sample—After blending, take the NOTE 3—An alternative method for the determination of total solids in
sample without delay. A suitable method is by slowly inserting synthetic rubber latex is described in Specification D 1076.
a clean, dry, glass tube of not more than 15 mm internal
5. Volatile Unsaturates (Residual Styrene)
diameter and open at both ends until it reaches the bottom of
the container. Then close the upper end of the tube and transfer 5.1 Scope—This test method measures the residual styrene
the contents to a clean, dry sample bottle. Repeat the operation of SBR synthetic rubber latices. It is not applicable to other
until sufficient latex has been obtained. synthetic rubber latices.
5.2 Apparatus:
NOTE 2—Alternatively, a specially constructed metal sampling tube 5.2.1 Iodine flasks having capacities of 250 cm3 each, and
may be used, the bottom of which can be closed by remote control. Copper distillation apparatus with ground-glass joints.
or brass must not be used in any part of its construction. 5.2.2 25-cm3 pipet.
3.3.3 Sample: 5.2.3 50-cm3 buret.
3.3.3.1 Where sub-samples are drawn from several contain- 5.3 Reagents:
ers, for example, 10 % sampling of latex in drums, or where 5.3.1 Synthetic Methanol, containing 100 ppm of p-tertiary
taken at different depths, for example from tanks, the sub- butyl catechol.
samples shall be combined and thoroughly blended by stirring 5.3.2 Standard Potassium Bromide-Potassium Bromate So-
lution (0.1 N)—Dissolve 2.784 g of potassium bromate
or shaking immediately before the final sample is taken.
(KBrO3) and 10.0 g of potassium bromide (KBr) in water and
dilute to 1000 cm3. Standardize with 0.1 N sodium thiosulfate
4. Total Solids
(Na2S2O3) solution in the presence of an excess (about 3 g) of
4.1 Apparatus: potassium iodide (KI) and sulfuric acid (H2SO4), (18 %).

2
 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
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D 1417 – 03
5.3.3 Sulfuric Acid Solution (18 %). 6. pH Value
5.3.4 Potassium Iodide Solution (10 %). 6.1 Apparatus—Any pH electrometer and a glass electrode-
5.3.5 Standard Sodium Thiosulfate Solution (0.1 N). calomel cell assembly may be used as described in Test
5.3.6 Starch Indicator Solution. Method E 70. A flowing calomel electrode has been found
5.4 Procedure: particularly suited for this use. The glass electrode shall be of
the type applicable for a pH range of from 2 to 14.
5.4.1 Weigh approximately 25 g of the latex to the nearest
6.2 Standard Solution—Use a standard solution having a pH
0.1 g in a tared, covered, 250-cm3 iodine flask. Remove the
of 10 or a standard solution having a pH approximately the
cover and add 25 cm3 of distilled water to the iodine flask. Add
same as that of the latex to be tested.
25 cm3 of synthetic methanol containing 100 ppm of p-tertiary
butyl catechol. Be sure to add the materials in the following 6.3 Procedure—Before making a determination take care
order: that the instrument is properly standardized at frequent inter-
vals with a standard solution (see 6.2), and that the electrodes
1. Latex. are clean. Permit the latex to come to equilibrium with the
2. Distilled water. glass electrode before taking the final reading. After the pH
3. Methanol containing p-tertiary butyl catechol. determination has been made, clean the electrodes thoroughly
5.4.2 Connect the iodine flask to the distillation apparatus and immerse them in distilled water. Report the pH value for
with ground-glass joints and distill the mixture. Collect the first the latex at a temperature of 25 6 2°C.
25 cm3 of distillate in a 250-cm3 iodine flask, rinse the
condenser with 20 cm3 of methanol containing 100 ppm of 7. Surface Tension
p-tertiary butyl catechol, and add the rinsings to the recovery 7.1 The surface tension of styrene-butadiene rubber latex
flask. shall be determined on the total solids of 40 6 1 %. If the
5.4.3 From a buret add 20 cm3 of 0.1 N standard KBr- viscosity is below 200 mPa·s (200 cP) on No. 1 spindle at 20
KBrO3 solution. Cool the solution to 30 C. Rapidly add 15 cm3 r/min, the latex can be tested with solids as received with little
of 18 % H2SO4 solution, stopper the flask, shake it, and add loss in accuracy.
distilled water to the funnel lips as a vapor seal. Allow the 7.2 Apparatus—Use a du Nouy tensiometer, carefully cali-
bottle to stand for 60 s. If no yellow color remains, add brated as described in Test Methods D 1331.
successive 10-cm3 portions of the bromide-bromate solution 7.3 Procedure—Strain approximately 25 cm3 of latex, ad-
until a slight yellow color persists for 60 s after the addition. justed to a temperature of 25 6 2°C, into a pan 60 to 65 mm
Make the additions by drawing the standard solution from the (2.4 to 2.6 in.) in diameter and 18 to 20 mm (0.7 to 0.8 in.) high
buret into the funnel lip and lifting the stopper so that the (Note 4). The surface of the latex must be free of air bubbles,
solution enters the flask around the stopper. Wash the funnel lip and the surface tension test shall be within 3 to 4 min to avoid“
with distilled water in the same manner and seal with water. skinning over” of the latex. Clean the tensiometer ring by
After 60 s has elapsed since the final bromide-bromate addi- heating in a bunsen flame. Extreme care must be taken to avoid
tion, add 10 cm3 of 10 % KI solution to the funnel lip, and lift distortion as the tensiometer ring is handled. Place the pan,
the stopper to allow the solution to enter the flask around the containing the latex being tested, beneath the ring on the
stopper. Shake the bottle and contents and titrate the liberated adjustable platform of the instrument. With the instrument
iodine with 0.1 N standard sodium thiosulfate solution to a adjusted so that the ring system is in its zero position when the
faint yellow color. Add 1 cm3 of starch indicator solution and ring is dry and the scale reading is zero, raise the platform until
continue the titration with sodium thiosulfate solution until the the latex makes contact with the ring. Submerge the ring
solution is clear. beneath the surface of the latex. Now slowly lower the
5.4.3.1 For a blank determination, repeat the procedure platform by means of the platform-adjusting screw and in-
using distilled water instead of latex. crease the torsion of the wire simultaneously, proportioning
5.5 Calculation—Calculate the percentage of volatile unsat- these two adjustments so that the torsion arm remains exactly
urates (residual styrene) as follows: in its zero position. As the film adhering to the ring approaches
Volatile unsaturates ~residual styrene!, % the breaking point, proceed more slowly with the adjustments
to make certain that the moving system is in its zero position
5 $@~D 3 E! 2 ~F 3 G!# 3 0.0521 3 100/M% 2 H (2) when the rupture occurs. The scale reading at which the ring
(2)
detaches from the latex represents, after proper correction, the
surface tension of the latex at the given temperature. Record
where: the average of three consecutive readings, discounting the first
D = cubic centimetres of standard bromide-bromate solu- reading. The ring is cleaned by flaming between readings and
tion used, all readings shall agree within 0.5 mN/m (0.5 dynes/cm).
E = normality of the bromide-bromate solution,
F = cubic centimetres of standard thiosulfate solution NOTE 4—The pan must be free of an oil film since traces of oil
introduce variable results in the surface tension measurement.
used for the titration,
G = normality of the thiosulfate solution, 7.4 Calculations—Calculate the surface tension, in
H = blank determination, %, and millinewtons/meter (dynes, per centimeter), as follows:
M = mass of latex used, g.
Surface tension, mN/m 5 M 3 N (3)

3
 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
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D 1417 – 03

where: 8.4.2 Start the agitator and evacuate the flask to 3.45 to 3.75
M = reading of the tensiometer, and kPa (approximately 1 in. Hg) or until the foam rises into the
N = a correction factor calculated as follows: neck of the flask. Break the vacuum. Evacuate several times in
this manner to ensure removal of the occluded air.
N 5 0.7250 1 =@~0.0003678 3 M!/R 2# 1 P (4)
8.4.3 Strain the deaerated latex through a 355-µm standard
where: screen. Determine the total solids content of the latex and then
M = reading of the tensiometer, accurately adjust the solids content of the latex to the desig-
R = radius of the ring, cm, and nated total solids content by the addition of distilled water. Add
P = a constant calculated as follows: the water slowly to the latex, and gently stir the mixture with
P 5 0.04534 2 ~1.679S/R! (5) a glass rod during the dilution.
8.5 Procedure:
where: 8.5.1 With the strained latex at a temperature of 256 2°C,
S = radius of the wire of the ring, cm, and pour the latex into the 600-cm3 beaker, taking care to avoid air
R = radius of the ring, cm. entrapment. Remove guard. This is done to reduce later
cleaning problems. Attach the spindle to the viscometer. Do not
8. Viscosity hit the spindle against the side of the beaker while it is attached
8.1 Scope—This test method covers the determination of to the viscometer as this can damage the shaft alignment. Lift
the viscosity of synthetic rubber latices using the Brookfield the shaft slightly and hold firmly with one hand while screwing
LV instrument for viscosities up to 2000 mPa·s (2000 cP) and the spindle on with the other hand. In most cases, spindle No.
the Brookfield RV instrument for viscosities of above 200 1 will give results in the required range. If not, change the
mPa·s (200 cP). spindle. Tilt the instrument slightly while immersing the
8.2 Summary of Test Method—The viscosity is determined spindle to avoid trapping air bubbles on the disk surface. Insert
by means of a viscometer that measures the torque produced on the spindle of the viscometer into the latex until the surface of
a specified spindle rotating at constant speed while immersed the latex is within the notch in the shaft of the spindle.
to a given depth in the latex. Alternatively, the spindle may be immersed in the latex in the
8.3 Apparatus: above manner before attaching it to the viscometer. Level the
8.3.1 Glass Stirring Rod. viscometer. Depress the clutch and turn on the viscometer
8.3.2 Screen—Standard sieve 355 µm. motor.
8.3.3 Distillation Flask, three-necked, equipped with a stir- 8.5.2 Select the speed of rotation of the instrument as
rer and vacuum connections. follows:
8.3.4 Beaker, having a capacity of 600 cm3. LV instrument: 6.3 rad/s (60 r/min)
8.3.5 Viscometer5—The viscometer shall contain an electric RV instrument: 2.1 rad/s (20 r/min)

synchronous motor capable of driving at a constant rotational 8.5.3 Measure 200 mL of latex in an 8-oz jar. Connect the
speed a shaft to which spindles of different shapes and guard and spindle #1 to the viscometer. Remember that the
dimensions may be attached. It shall contain a scale and a spindle has a left-hand thread and must be screwed firmly into
pointer, which will indicate the equilibrium torque developed place.
by the resistance to rotation of a spindle properly immersed in
latex. A bubble level shall be incorporated in the motor housing NOTE 5—Always lift up on the spindle when attaching it to the
viscometer. This is done to avoid damage to the instrument’s pivot point
to indicate, with the spindle attached to the motor shaft, when and jewel bearing.
the spindle is vertical. The viscometer must not contain a foot
bearing, because of possible interference due to coagulum Place the 8-oz jar on the platform jack under the viscometer.
formation on the bearing. Raise the jar to the guard and spindle. Hold the jar at an angle
8.4 Preparation of Sample: to prevent air bubbles from being trapped under the spindle.
8.4.1 If the latex contains occluded air, remove the air in the Adjust the height of the latex to the groove on the spindle. Set
following manner before proceeding with the determination of the spindle speed to 60 rpm on the left side of the viscometer.
viscosity. After diluting the latex (if viscosity is to be deter- When the sample is ready to be analyzed, hold down the toggle
mined at lower designated solids) with distilled water to the switch on the back of the viscometer and turn on the power
approximate desired total solids, pour a sufficient volume of switch on the right. After the power is on, the toggle switch
the latex into a three-necked distillation flask equipped with a may be released. Let the viscometer stabilize for approximately
stirrer and vacuum connections so that at least 500 cm3 of latex 60 s. To obtain the reading, hold down the toggle switch and
will remain after the removal of the air. then turn the power switch off when the red needle stops in the
window. The red needle points to the viscosity in units of
centipoise (cps). Repeat Steps 7 and 8 at least three times to
find an average reading. Report the viscosity to the nearest 1
5
The sole source of supply of Brookfield Viscometers, Models LVF, LVT, RVF, cps.
RVF-100, and RVT known to the committee at this time is Brookfield Engineering,
Inc., Stoughton, MA 02072. If you are aware of alternative suppliers, please provide
8.6 Calculation—For spindle No. 1 and 60 r/min:
this information to ASTM International Headquarters. Your comments will receive RDG.X 1 5 cps (6)
careful consideration at a meeting of the responsible technical committee 1, which
you may attend. NOTE 6—If it is desired to better characterize the latex, additional

4
 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 1417 – 03
rotational speeds may be used. while under fast agitation. The resulting crumb is filtered,
dried, and massed on a rubber mill. The viscosity of the
9. Coagulum Content
contained polymer is measured in a shearing disk viscometer.
9.1 Apparatus: 11.3 Apparatus:
9.1.1 Nylon filter cloth, 25 micron. 11.3.1 Blendor6—Explosion-proof type.
9.1.2 Beaker, tared. 11.3.2 Cheesecloth.
9.1.3 Demineralized Water (DMW). 11.3.3 Drying Tray, approximately 30 by 20 by 2.5 cm (12
9.1.4 Air Oven. by 8 by 1 in.) with a 1.00 to 1.41 mm mesh plastic screen
9.1.5 Desiccator. supported by a coarse screen bottom.
9.2 Procedure—Store clean nylon (25 micron mesh) filter 11.3.4 Draft Oven, maintained at 125 6 2°C.
circles (9.0 6 0.2 cm in diameter) in a desiccator. Weigh the 11.3.5 Laboratory Mill, as described in Practice D 3182.
clean filter and record this weight to four decimal places. Place 11.3.6 Shearing Disk Viscometer, as described in Test Meth-
the filter on the porcelain Buchner funnel; set the funnel on a ods D 1646.
2000-mL flask. Weigh 500 6 0.5 g of latex sample into a 11.4 Reagents and Materials:
1200-mL beaker. Add 500 6 1 mL of DMW and stir gently. 11.4.1 Sodium Chloride Solution (250 g/dm3)—Dissolve
Filter the sample through the nylon filter with the aspirator 250 g of ACS Grade NaCl in 1 dm3 of demineralized water.
slowly. If drainage stops, use a plastic pipet and gently swirl 11.4.2 Methanol Solution (7.5 g/dm3)—Dissolve 7.5 g of a
the liquid in a whirlpool fashion slowly, taking care not to suitable antioxidant7 in 1 dm3 of USP methanol.
touch the nylon filter on the bottom of the liquid. This usually 11.4.3 Sulfuric Acid (1 + 9)—Add 100 cm3 of concentrated
allows drainage to resume. Rinse the filter gently with squirts ACS Grade H2SO4(sp gr 1.84) to 900 cm3 of demineralized
of DMW (50 mL). All latex must be rinsed through the filter. water.
Dry the filters in the 70°C blue M oven for 15 min. 11.4.4 Congo Red Indicator Paper.
NOTE 7—Take care not to lose any floc in transferring from oven to 11.4.5 Agerite White (KD-64 Harwick) stock dispersion
counter to balances. Cool the filter for 15 min in a desiccator. Weigh the 11.4.6 2.2 % Aluminum Sulfate, dissolve 378 grams in 5
filter plus residue to four (4) decimal places. Calculate and report the gallons of tap water and agitate vigorously. Some precipitate
residue to the nearest third decimal place [Spec:0.010 % maximum]. will remain in the reagent.
9.3 Calculation: 11.5 Procedure:
11.5.1 Coagulation Procedure—If the total solids content of
~Weight of filter& residue! 2 ~Weight of filter!
5 5 % Residue the latex is greater than 30 %, dilute the latex with distilled
(7) water to a total solids contents of approximately 30 %. Add to
250 cm3 of the diluted latex, 50 cm3 of the NaCl solution and
For a 500 gram sample: mix thoroughly.
~Weight of filter & residue! 2 ~Weight of filter! 11.5.1.1 Add 250 cm3 of methanol-anti-oxidant solution
5 % Residue (8)
5 while continuing to agitate. Add 10 cm3 of H2SO4(1 + 9)
NOTE 8—When mechanically concentrated latices are tested, use dis- slowly during a period of 2 to 3 min. If the coagulating solution
tilled water as the diluent. does not turn Congo Red paper from red to blue, add additional
H2SO4 while stirring until the color does change.
10. Determination of Bound Styrene in Contained 11.5.1.2 Pour the contents of the coagulating cup onto
Polymer cheesecloth and press as much serum as possible from the
10.1 Scope—This test method is designed to measure the mass. Hand separate the mass, wash it thoroughly with
bound styrene content of butadiene-styrene copolymers. The demineralized water, and transfer the pieces to a drying tray.
test method is not applicable when a high styrene latex (above 11.5.2 Drying Procedure—Dry the crumb in a draft oven at
50 % bound styrene) is a component of the latex system. 125 6 2°C. Drying time will vary with the crumb consistency,
10.2 Coagulation Procedure—Use the test method outlined polymer Mooney viscosity, and oven conditions and should be
in 11.5. determined by experimentation. Drying time shall be deter-
10.3 Bound Styrene Determination—Use the test method mined by reference to a volatile matter versus time plot. The
described in Test Methods D 1416. desired drying time shall be taken at a time less than 5 min after
the minimum level has been reached. Over drying and under
11. Determination of Mooney Viscosity of Contained drying will both give incorrect Mooney viscosity values and
Polymer are to be avoided.
11.1 Scope—This test method is designed to measure the 11.5.3 Determination of Mooney Viscosity—Mill mass the
viscosity of the contained polymer of anionic stabilized syn- rubber and determine the Mooney viscosity in accordance with
thetic rubber latices having a residual monomer content of less Test Methods D 1646.
than 0.50 % by weight. It is not applicable to latices of
polymers containing substitute carboxylic acid groups on the
6
polymer chain, hot polymerized BR (2004), CR, NCR, SCR, or A Model FCI-15 Waring Blendor, or equivalent, has been found satisfactory for
this purpose.
ABR. 7
Antioxidants of the bis or polyphenol types such as Ethyl 702, Santowhite
11.2 Summary of Test Method—The latex is coagulated by Powder, and Wingstay L, and of the diaryl-p-phenylenediamine type such as
the consecutive addition of salt, methanol, and acid solutions Wingstay 200, have been found to be equivalent to PBNA.

5
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D 1417 – 03
11.5.4 Special Procedure for Vinylpyridine latex (PSBR): The shaft shall run with not more than 0.25 mm (0.010 in.) out
11.5.4.1 Coagulation of Latex—Add 2400 ml of warm of true at the speed specified.
water (130°F) to the container and start agitation. Add 25 ml of 12.3.2 Agitator Disk—The agitator itself shall consist of a
Agerite White Dispersion. Add 200 ml of latex to be tested (or polished stainless steel disk 36.12 6 0.03 mm (1.4226 0.001
sufficient to provide 75–80 grams of polymer). Increase agita- in.) in diameter and 1.58 6 0.05 mm (0.062 6 0.002 in.) in
tion and slowly add 2 % aluminum sulfate (increase agitation if thickness having a threaded stud at its exact center for
coagulated polymer starts to form a ball) until coagulation is attachment to the center of the lower end of the stirrer shaft.
complete. This can be determined by observing the serum. The 12.3.3 Test Bottle—The test bottle shall be a flat-bottom
serum solution will be relatively clear and contain a few very cylindrical glass container 57.8 6 1 mm (2.28 6 0.04 in.) in
fine particles when coagulation is complete. Continue agitation inside diameter by approximately 12.7 cm (5 in.) in height, and
for one (1) minute after complete coagulation. Allow to stand having a wall thickness of approximately 2.3 mm (0.09 in.).
for 10 minutes. Seperate the crumb from the serum by filtering 12.3.4 Bottle Holder—The bottle holder shall be so con-
through a fine, lint-free cloth. structed that the bottle may be conveniently lowered and raised
11.5.4.2 Drying—The coagulum during filtration may tend to the exact specified position with relation to the shaft and
to agglomerate into a mass. Break this mass into very small agitator. The position of the test bottle shall be such that the
pieces. Dry the crumb in an air oven at 90°C. When the crumb axis of the stirrer shaft is concentric with the axis of the bottle
is dry, it will completely lose its white color and turn brown. and that the bottom of the agitator disk is 12.7 6 2 mm (0.5 6
This should require 11⁄2 to 21⁄2 hours. Check for dryness after 0.1 in.) from the bottom inside of the bottle.
one (1) hour drying time and every 15 minutes thereafter til 12.3.5 Stainless Steel Screen—No. 180 µm sieve with 0.180
dry. Remove when dry. To determine if the crumb is dry, pull 6 0.009-mm (0.0070 6 0.0004-in.) opening and 0.131 6
several pieces apart and, if any white shows, dry for an 0.01-mm (0.0052 6 0.0005-in.) wire diameter. The screen
additional 1⁄2 hour. Do this until the crumb is completely dry. shall be cut to fit into the seat of a pipe union having inside
11.5.4.3 Milling of Crumb—Using the sample prepared in diameter of about 5 cm (nominal 11⁄2-in. pipe size).
10.4.2 above, mass the crumb together into a ball in your 12.4 Procedure:
hands. Ensure that the dry crumb is at least 60 grams. Set mill 12.4.1 If the viscosity of the latex as determined by Section
temperature at 8565°F and the distance between rolls at 8 of this test method is greater than 350 mPa·s (cP), dilute the
0.06560.005 inches. With the speed set at 40 rpm, pass the latex with sufficient water so that the viscosity is below 350
sample through the mill ten times, doubling it during passes 2 mPa·s (cP), except that in no case should the latex solids be
through 9. Do not band the material, or let it stick to the rolls reduced by more than 10 % relative.
so that it is carried around. It may be necessary to actually stop 12.4.2 Strain the latex through a 180-µm sieve and weigh 50
the mill after each pass in order to make seperate, independent 6 0.5 g of the strained latex into the test bottle. Place the bottle
passes. Allow the milled samples to sit for thirty minutes at containing the latex in the holder of the stability tester.
room temperature before testing. 12.4.3 Start the tester and agitate for exactly 30 min (or
11.5.4.4 Determination of Mooney Viscosity—After the other agreed-upon time) at 1470 6 21 rad/s (14 000 6 200
sample has been prepared as detailed above, run the Mooney r/min). The time of agitation should be adjusted so that the
test as listed in ASTM D 1646, Paragraphs 9–12. temperature of the latex does not increase to more than 60°C.
Remove the sample immediately to avoid any filming and rinse
12. Determination of Mechanical Stability the agitator shaft and disk with distilled water. Strain the latex
12.1 Scope—This test method covers the determination of through a tared 180-µm screen that has previously been wetted
the stability of synthetic latices when subjected to highspeed with a 2 % aqueous solution of a surfactant such as potassium
mechanical stirring. oleate. Finally, flush the screen with the same solution and then
12.2 Summary of Test Method—A sample of latex is sub- follow with a rinse of distilled water. Dry the screen and
jected to mechanical shear by the use of a high-speed stirrer coagulum in a force draft oven at 100 6 2°C to constant mass
and the extent of instability noted. The amount of coagulum (approximately 15 min). Cool and weigh again to 60.001 g.
formed after a given time of agitation is considered a measure 12.5 Calculation—Calculate the percent coagulum as fol-
of latex instability. lows:
12.3 Apparatus: Coagulum, % 5 [~A 2 B!/50] 3 100 (9)
12.3.1 Tester5,8—The test apparatus shall consist of a ver-
tical shaft high-speed stirrer capable of maintaining a speed of where:
A = mass of tared screen plus coagulum, and
14 000 6 200 r/min for the duration of the test. The stirrer shaft
B = mass of tared screen.
shall be approximately 6.3 mm (0.25 in.) in diameter at its
12.6 Report—Report the percent coagulum, the total solids
lower end at the point of attachment of the agitator disk and
content at which the latex was tested, and the duration of
may taper upward for greater strength. It shall be of sufficient
stirring, in minutes.
length to reach conveniently to the bottom of the test bottle.
12.7 Mechanical Stability of Latex (Alternate method)
12.7.1 Scope—This method determines the amount of latex
which is coagulated under shearing conditions of the test. A
8
The sole source of supply of the apparatus known to the committee at this time sample of latex is subjected to mechanical shear by the use of
is Custom Scientific Instruments, Inc., 13 Wing Dr., Whippany, NJ 07981. a high speed stirrer and the extent of instability is noted. The

6
 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 1417 – 03
amount of coagulum formed after a given time of agitation is 13. Determination of Polystyrene Reinforcement in
considered a measure of latex stability. Contained Polymer
12.7.2 Equipment: 13.1 Scope—This test method is designed to measure the
1. 200 mesh screen polystyrene content of polystyrene-reinforced SBR latices in
2. 80 mesh polyester screen the range from 1 to 100 % polystyrene. The test method is not
3. 100 ml graduated cylinder applicable on polymers containing gel, unless it has been
4. Hamilton Beach Drinkmaster No. 30 proven that gel does not interfere.
5. Plastic seal for the mixer cup (1 qt) 13.2 Procedure—Determine the polystyrene content in ac-
6. Clamp, screw chain cordance with Test Method D 3314.
7. Microwave oven
12.7.3 Procedure—Cool the latex to 100°F if it is found to 14. Determination of Residual Acrylonitrile Content
be above this temperature. Filter approximately 170 ml of latex 14.1 Scope—This test method measures the residual acry-
through a 200 mesh screen. Pour 150 ml of this latex into the lonitrile content of nitrile rubber latices that have a residual
mixer cup. To eliminate air drying, place the plastic seal over acrylonitrile content of less than 0.2 %.
the mixer cup and secure with the chain clamp while the test is 14.2 Summary of Test Method—The latex is distilled and the
running. Agitate on the Hamilton Beach mixer for 30 minutes distillate is collected in methanol. n-Dodecyl mercaptan is
at the “low” setting. Preweigh an 80 mesh polyester screen. At added to the distillate and the excess is titrated with iodine
the conclusion of the test, inspect the sample for air dried latex. solution.
If any is found, dispose of the sample and rerun, making sure 14.3 Apparatus:
that the seal is tight. Immediately after removing the mixer cup, 14.3.1 Distillation Apparatus, consisting of a 500-cm3 dis-
pour the latex through the preweighed 80 mesh polyester tillation flask, still head, vertical water-cooled condenser, and
screen. Wash the residue from the cup through the screen using 100-cm3 receiver with glass stopper through which pass a glass
additional wash water. Dry to constant weight using micro- tube connected to the condenser and a shorter exit glass tube
wave oven. Reweigh the screen containing the dried coagulum leading into a 50-cm3 beaker.
and find by difference the amount of coagulum collected. 14.3.2 Volumetric Flask, 100-cm3.
Express the final results in ppm as shown below: 14.3.3 Conical Flask, at least 250-cm3.
Grams Coagulum 14.4 Reagents:
150 3 1,000,000 5 ppm Residue (10) 14.4.1 Purity of Reagents—Reagent grade chemicals shall
be used in all tests. Unless otherwise indicated, it is intended
12.8 Centrifuge Stability
that all reagents shall conform to the specifications of the
12.8.1 Scope—This method was designed to readily predict
Committee on Analytical Reagents of the American Chemical
creaming stability of vinylpyridine containing latices. The
Society, where such specifications are available.9 Other grades
amount of agglomerated cream is determined after diliting,
may be used, provided it is first ascertained that the reagent is
centrifuging and filtering.
of sufficiently high purity to permit its use without lessening
12.8.2 Equipment: the accuracy of the determination.
1. Centrifuge, Sorvall GLC1 or equivalent, at least 2500 rpm 14.4.2 Purity of Water—Unless otherwise indicated, refer-
2. Centrifuge jars, 100 ml with caps ences to water shall be understood to mean distilled water or
3. Jars, 1 quart, wide mouth, with lids water of equal purity.
4. Balance, 3000–gram capacity 14.4.3 Acetic Acid, glacial (CH3COOH).
5. Balance, Analytical 6 0.1 mg 14.4.4 n-Dodecyl Mercaptan, Alcoholic Solution
6. Screen, 325 mesh, to fit residue holders (1.25 %)—Dissolve 12.5 g of n-dodecyl mercaptan
12.8.3 Procedure: (CH3(CH2)11SH) in 500 cm3 of 2-propanol dilute to 1000 cm3.
12.8.3.1 Mix the latex well and filter through a paint 14.4.5 Iodine Solution (0.0125 M)—Transfer 3.2 g of iodine
strainer. Dilute the amount of latex obtained from from the and 15 g of potassium iodide (KI) to an 800-cm3 beaker, add 30
formula listed in 13.4.1 below to 900 grams with deionized ml of water, and stir until all solution is complete. Dilute with
water and mix well. Immediately transfer 100 ml of the diluted water to 500 cm3, and filter through a sintered-glass filter. Wash
latex to a 100 ml centrifuge jar. Make certain that the jar is the filter with about 15 cm3 of water, transfer the combined
clean and dry. Centrifuge the 100 ml sample at 2200 rpm for 1 filtrate and washing to a 1000-cm3 volumetric flask, dilute to
hour. After centrifuging, pour the liquid through a tared 325 the mark with water, and mix. Store the solution in a glass-
mesh screen. Rinse the jar several times, pouring each rinse stoppered, amber-glass bottle in a cool place. Standardize with
through the filter. Dry the screen in a microwave over for 3 sodium thiosulfate.
minutes on high and weigh. Record the weight of residue as 14.4.6 Methanol (CH3OH).
specified by the calculation listed in 3.4.2 below.
12.8.4 Calculations:
900 3 30 9
Reagent Chemicals, American Chemical Society Specifications, Am. Chemical
Grams of latex to dilute 5 TSC (11) Soc., Washington, DC. For suggestions on the testing of reagents not listed by the
American Chemical Society, see Reagent Chemicals and Standards, by Joseph
Rosin, D. Van Nostrand Co., Inc., New York, NY, and the United States Pharma-
Grams of residue 3 10,000 ppm 5 residue in ppm (12) copeia.

7
 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 1417 – 03
14.4.7 Potassium Hydroxide, Alcoholic Solution (6 %)— B = iodine solution used in the blank determination, cm3,
Grind 6 g of potassium hydroxide (KOH) with successive C = iodine solution used in the sample titration, cm3,
25-cm3 portions of 95 % ethanol until dissolution is complete. D = aliquot of dilute distillate, cm3,
Dilute to 100 cm3 with 95 % ethanol. Filter immediately into a E = 2 milliequivalents of iodine per millimole of iodine,
dark bottle and keep tightly closed. Let this solution stand F = 0.05306 of acrylonitrile per millimole,
overnight before using. When it becomes noticeably discol- M = mass of sample, 25 g, and
ored, it should be discarded. Storing in a nitrogen atmosphere V = total volume of distillate, 100 cm3.
will preserve the solution considerably. The results of duplicate determinations shall agree within
14.4.8 2-Propanol ((CH3)2CHOH). 0.005 % absolute.
14.4.9 Sodium Carbonate (Na2CO3).
15. Particle Size Determination
14.4.10 Sodium Thiosulfate Solution (0.0125 M)—Dissolve
3.1 g of sodium thiosulfate (Na2S2O3·5H2O) in 500 cm3 of 15.1 Apparatus:
freshly boiled and cooled water, and add 0.1 g of sodium 15.1.1 Malvern Autosizer:
carbonate (Na2CO3). Dilute to 1000 cm3 with freshly boiled 15.2 Procedure:
and cooled water, and let stand for 24 h. Store the solution in 15.2.1 Turn on Malvern Autosizer 2c for warm-up. Warm
a tightly closed glass bottle. Standardize in accordance with the up for two minutes. Select option nine from starting menu
procedure in Practice E 200. program on computer. Make sure temperature on Malvern is
14.4.11 Silicone Antifoam Agent. 25°C or 60.2. Adjust if needed. Make sure beam size on
14.5 Procedure: Malvern is set to small. Select F2 for sample description;
14.5.1 Weigh 25.0 6 0.2 g of latex into the distillation flask follow screen instructions. Toggle F5 key for results printout
and add 100 cm3 of water and 1 cm3 of a suitable silicone option.
antifoam agent. Place 25 cm3 of methanol in the receiver and 15.3 Preparation of Sample:
approximately 10 cm3 of methanol in the 50-cm3 beaker. 15.3.1 Using a 5-mL syringe, filter 20 mL DMW into a
Assemble the distillation apparatus so that the end of the tube clean 50-mL beaker using a corning disposable sterile syringe
connected to the condenser is immersed in the methanol in the filter. Also with the syringe, filter DMW into a four-sided
receiver and the end of the exit tube connected to the receiver cuvette to 2⁄3 full capacity. Using a disposable pipette, add one
is immersed in the methanol in the 50-cm3 beaker. (The drop of latex to the 50-mL beaker. Swirl beaker until solution
purpose of the 50-cm3 beaker is to recover any distillate not is uniform. Using a disposable pipette, transfer three drops of
collected in the receiver.) Immerse the receiver and 50-cm3 solution into the cuvette. Cover top with a small piece of
beaker in ice. parafilm and shake for a few seconds. Remove parafilm and
14.5.2 Distill the mixture, adjusting the rate of boiling to insert a plastic cuvette top snugly. Place sample in Branson
control frothing, and collect 50 cm3 of distillate in the receiver. 1200 ultrasonic cleaner and sonicate for 30 s. Remove sample
14.5.3 Empty the contents of the receiver and 50-cm3 and dry outside of cuvette with a Kimwipe. Place cuvette into
beaker into the 100-cm3 volumetric flask. Rinse twice with autosizer machine and close door (beam size—SMALL).
about 5 cm3 of methanol by pouring the methanol through the 15.4 Analysis of Sample:
condenser into the receiver and add the washings to the 15.4.1 Adjust counts/1000 using the dial on top of the
volumetric flask. Dilute to the mark with methanol. autosizer. Adjust to approximately 100. Sample level should be
14.5.4 Pipet a 50-cm3 aliquot of the diluted distillate into the near “ideal.” If not, adjust very gently with beam dial (near
conical flask that contains 25 cm3 of 2-propanol. Pipet 10 cm3 150) or dilute the latex sample. If printout is desired, make sure
of mercaptan solution into the flask. Add 1 cm3 of alcoholic printer ribbon is even with top of page. Printer: Power, ready,
potassium hydroxide and allow the solution to react for exactly and on-line lights should be illuminated. F4 key starts sample
2 min at 23 6 2°C. Add 2 cm3 of glacial acetic acid to stop the measurement. Printout starts after about 4.5 min. Printing lasts
reaction. The resulting pH value should be between 4 and 6. for approximately 1 min. The Z average mean value at the end
Titrate with freshly standardized iodine solution to a yellow of the printout is recorded as particle size. Space key returns
color that persists for at least 60 s. Discard the iodine solution user to menu screen. E exits program. Turn off Malvern
remaining in the buret, unless it is required for immediate use. instrument.
14.5.5 Run a blank determination, omitting the distillation
16. Bound Monomers in Vinylpyridine Latex
stage, using 50 cm3 of 50-50 methanol-water mixture.
14.6 Expression of Results—Calculate the residual acryloni- 16.1 Scope—This test method covers the range of vinylpy-
trile content as a percentage by mass of the latex as follows: ridine, styrene and butadiene normally encountered with vi-
nylpyridine containing latices. It is not applicable to other
A 3 ~B 2 C! 3 V 3 E 3 F
D3M 3 100 (13) synthetic latices. This method utilizes the infrared absorption
bands at 1490, 1470 and 910 cm –1 wavenumbers arising from
which simplifies to: C = C stretching modes in styrene and vinylpyridine and
A 3 ~B– C! 3 0.424 CH=CH2 bending of the vinyl groups of polybutadiene seg-
Residual acrylonitrile, % 5 3 100 (14)
D ments, respectively. Because only absorption ratios are used in
the calculations, the need to determine film thickness is
where: eliminated.
A = molarity of the iodine solution,
16.2 Apparatus:

8
 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 1417 – 03
16.2.1 Double beam infrared spectrophotometer, Model 283 2. Column P&E 10 % apiezon L on 80/100 chromosorb W,
or equivalent. or Supelco 10 % SP 2100 and 80/100 Supelcoport.
16.2.2 KRS-5 crystals - 25 3 4 mm 3. Capsule sampler - Model MS-41
16.2.3 Crystal holder 4. Capsules, capsule holder
16.2.4 Applicator sticks 5. Filter paper, No. 5
16.3 Procedure: 6. Micropipetter, 1 µl - Fisher No. 21-170-10
16.3.1 Place a drop or two of latex on a KRS-5 crystal. 7. Micropipettes, for Micropipetter above, 1 µl, Fisher No.
Spread the latex evenly over the entire crystal as quickly as 21-170-11
possible with an applicator stick. Allow to dry under a heat 8. Absorbent tissues, Kimwipes, or equivalent
lamp for 3–5 minutes. The film thickness should be such that 9. Cork bore, No. 1
all absorbance values remain on scale using an expansion 10. Integrator, Model 2, Spectraphysics
factor of 1 to 1.5x. Use the following instrument parameters:
11. Syringe, Pressure-Lok, 2 ml
scan time = 60 minutes, response setting = 2, slit setting = 7,
12. Pressure bottle, 8 ounce with Teflon lines septum cap
absorbance mode, gain = full counterclockwise. Scan over the
wavelength regions 1550–1450 cm−1 and 950–850 cm−1. Clean 13. Analytical balance
the crystals with Tetrahydrofuran solvent. Repeat the procedure 17.3 Reagents:
two more times, so that triplicate analyses are obtained. 1. Gases: –Helium, the regulator outlet pressure should be set at 70 psig.
–Hydrogen, the regulator outlet pressure should be set at 20 psig.
16.4 Calibration: – Plant air, the regulator outlet pressure should be set at 35 psig
16.4.1 Obtain styrene-butadiene-vinylpyridine latices where on No.1 and 2 (Model 3920) and No. 3 (Sigma 2) instruments. All
the bound monomers are accurately known. At least two gases must be of prepure quality.
2. Volatile Standard, 99.9 % purity
different levels of vinylpyridine are needed. The following a. Butadiene
relationships are used for the calibrations: b. 4-Vinylcylcohexane
c. Ethlybenzene
C styrene A1490 d. Styrene
CVP 5 a 1 b A1470 (15) e. Vinylpyridine
f. Other monomers and solvents as requested
3. Control latex with known level of styrene.
Cstyrene A1490 4. Solvent, carbon disulfide (CS2), chromatographic grade.
CBD 5 g 1 h A910 (16) 5. Methyl alcohol, chromatographic grade

17.4 Procedure:
Cstyrene 1 CVP 1 CBD 5 100 (17) 17.4.1 Capsulating the Sample:
where: 17.4.1.1 Using forceps, transfer a capsule to a 10 capsule
Cx = wt. % values for the given monomer magazine. The capsule must fit securely. Use new plastic
Ax = absorbance at wavelength X magazine inserts if the capsule is not held securely. Using a No.
Constants a, b, g and h are then determined from a series of 1 cork bore, cut out a piece of filter paper and insert in the
standard latices containing different known levels of the bottom of the capsule. Place the capsule magazine in the
monomers. Concentration values for vinylpyridine can also be sealing unit with the capsule opposite the cutting blade.
obtained by determining total nitrogen content using the Loosening the knurled knob on the micropipettor, carefully
Kjeldahl or Dumas procedures (preferably the latter). How- insert a micropipette and tighten the knurled knob securely.
ever, to use the total nitrogen methods requires that no other Depress the plunger and insert the pipette into the sample. With
nitrogen containing compounds be present. the pipette still in the sample, release the plunger. The sample
16.5 Calculation: will be in the micropipette. Remove the pipette from the
16.5.1 After the four constants listed above (a, b, g and h ) sample. Wipe the outside of the pipette with a tissue. Discharge
are determined, the three equations listed in 5.4.1 above can it into the capsule, touching the filter paper. Quickly seal the
then be solved simultaneously. A computer program can be set capsule by pulling down on the crimping lever. The sealed
up to perform these calculations. capsule in the magazine is then transferred to the capsule
holder using the capsule loading unit.
17. Residual Monomers 17.4.2 Injection of the Sample:
17.1 Scope—This method describes the operation of the 17.4.2.1 For Model 3920: Remove the capsule holder from
Perkin Elmer gas chromatograph. This instrument is used to the hot injector assembly and immediately align the capsule
test for residual monomers in the latex, as well as the purity of holder in the loading unit with capsule in the magazine. Press
the raw material. The use of the sample encapsulating unit is down on the capsule holder firmly until the capsule is seated in
described. The method can be applied to any liquid sample and the capsule holder. Be certain to remove any used capsule from
many solis samples provided the proper columns and condi- the holder and instrument. Remove the capsule holder from the
tions are used. This preferred method is Test Method D 4026 – loading unit. Check for the conditions desired, and wait for the
Method B. This method may not give the same results as the green light to come on. The green light must be on before
wet method. inserting the sample. Gently and slowly insert the capsule
17.2 Equipment: holder containing the sample capsule, just short of puncturing
1. Perkin Elmer gas chromatograph, Model 3920 or Sigma 2, the capsule. The capsule should be in the injection port to be
with FID heated. After 15 seconds, insert the capsule holder all the way

9
 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 1417 – 03
into the instrument to puncture the capsule. The forepart of the monomer in the syringe should be vented to the outside air. The
capsule holder will be almost flush with the front of the pressure bottle of Bd should also be vented to the outside air
instrument. Immediately after injecting the sample, press the after standards have been tested. The samples are ready to be
start button on the integrator. Do not press the light on the injected into the Gas Chromatograph.
chromatograph. After one minute, remove the capsule holder
from the instrument. While the instrument is cooling, reinsert 18. Precision and Bias
the capsule holder to keep it hot. When the door opens at the 18.1 This precision and bias section has been prepared in
end of the testing cycle, press the button again to stop the accordance with Practice D 4483. Refer to Practice D 4483 for
integrator. Turn off the chart. When the instrument has cooled terminology and other statistical calculation details.
to the initial temperature, another sample can be injected. The 18.2 The precision results in this precision and bias section
integrator prints out the elution time and the peak area, and the give an estimate of the precision of these test methods with the
ppm of each component of interest. materials (rubbers) used in the particular interlaboratory pro-
17.4.2.2 For Model Sigma 2: Set instrument for conditions gram as described below. The precision parameters should not
desired, and wait for the oven ready light to come on. This light be used for acceptance/rejection testing of any group of
and the start button must be lit before injecting the sample. materials without documentation that they are applicable to
Gently and slowly insert the capsule holder containing the those particular materials and the specific testing protocols that
sample into the instrument, just short of puncturing the capsule. include these test methods.
The capsule should be in the injection port section to be heated. 18.3 A Type 1 (interlaboratory) precision was evaluated.
After 15 seconds, insert the capsule holder all the way into the Both repeatability and reproducibility are short term; a period
instrument to puncture the capsule. The forepart of the capsule of a few days separates replicate test results. Information on the
holder will be almost flush with the front of the instrument. number of laboratories and the materials used is given in Table
Immediately after injecting the sample, press the start button 2.
on the instrument. This starts the instrument and the computer.
18.4 The results of the precision calculations for pooled
At the end of the cycle, the oven will cool and the results will
repeatability and reproducibility are given in Table 2 for a
be printed out. When the instrument has cooled to the initial
broad series of test parameters.
temperature, another sample can be injected.
18.5 The precision of these test methods may be expressed
17.4.3 Preparation of Standards for Instrument Standard-
in the format of the following statements which use an
ization:
“appropriate value” of r, R, (r), or (R), to be used in decisions
17.4.3.1 Liquid Monomers (Styrene, VP, etc): Place 100 ml
about test results. The appropriate value is that value of r or R
of carbon bisulfide in the pressure bottle and seal tightly.
associated with a mean level in Table 2 closest to the mean
Transfer approximately 2 ml of monomer into a Pressure-Lok
level under consideration at any given time for any given test,
syringe and close the valve. Expel any air. Make certain the
for any given material in routine testing operations.
syringe does not leak. Using an absorbent tissue, clean the
18.6 Repeatability—The repeatability, r, of these test meth-
outside of the syringe and weigh. Carefully inject the required
ods has been established as the appropriate value tabulated in
amount of monomer into the pressure bottle below the liquid
Table 2. Two single test results, obtained in two different
surface and mix. Withdraw the syringe and re-weigh. Follow
laboratories, under normal test method procedures, that differ
the above procedure for each addition of monomer. The
by more than the tabulated r (for any given must be considered
syringe may have to be refilled. Any excess monomer should
to have come from different or nonidentical sample popula-
be expelled into a solvent waste safety can for proper disposal
tions.
and the syringe should be rinsed copiously with methyl alcohol
and allowed to air dry. 18.7 Repeatability and reproducibility expressed as a per-
17.4.3.2 Butadiene (Bd): Obtain a small sample of butadi- cent of the mean level, (r) and (R), have equivalent application
ene (liquid) and place it on dry ice. Place a 2 ml Pressure-Lok statements as above for r and R. For the (r) and (R) statements,
syringe in the freezer and allow it to come to freezer tempera- the difference in the two single test results is expressed as a
ture. Place 100 ml of carbon disulfide in the pressure bottle(s) percent of the arithmetic mean of the two test results.
to which other monomers have been added. Store in the freezer 18.8 Bias—In test method terminology, bias is the differ-
and allow to come to temperature. Transfer the Bd to the ence between an average test value and the reference (or true)
syringe and close the valve. Using an absorbent tissue, clean test property value. Reference values do not exist for these test
the outside of the syringe, place in an insulator tube and weigh. methods, since the value (of the test property) is exclusively
Carefully inject the required amount of monomer into the defined by the test methods. Bias therefore cannot be deter-
pressure bottle below the liquid surface and mix. Withdraw the mined.
syringe, place in an insulator tube and re-weigh. The difference
is the amount of Bd injected. Prepare standards at about 0.01, 19. Keywords
0.04, 0.1, 0.3 and 0.7 grams per 100 ml of solvent. Any excess 19.1 latex; rubber latices; synthetic

10
 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 1417 – 03
TABLE 2 Type 1 Precision for Synthetic Rubber Latices—Various Tests

NOTE—Midpoint of range used for (r) and (R) calculations:

Sr = Repeatability standard deviation, in measurement units,

r = Repeatability, in measurement units,
(r) = Repeatability, (relative) percent,
SR = Reproducibility standard deviation, in measurement units,
R = Reproducibility, in measurement units, and
(R) = Reproducibility, (relative) percent.
Property Range Within Laboratory Between Laboratories Number of Number of
Tested Property Participat-
Test Method
Sr r (r) SR R (R) Levels ing Labora-
tories
Total solids, % 29.40 to 67.3 0.06 0.17 0.35 0.08 0.23 0.47 4 4
Volatile unsaturates, % 0.012 to 0.12 0.007 0.020 30.3 0.011 0.031 47.0 4 4
pH value 9.52 to 10.50 0.05 0.142 1.4 0.11 0.311 3.1 4 5
Surface tension, Mn/M 31.8 to 51.2 0.30 0.85 2.1 0.80 2.26 5.5 4 3
Viscosity, mPa·s, 6.0 to 40.3 0.40 1.13 4.9 1.60 4.53 19.6 3 4
Coagulum content mass 0.000 to 0.0320 0.00050 0.0014 9.4 0.0053 0.015 99.0 4 3
(weight), %
Mooney viscosity, 52.6 to 192.0 3.4 9.62 7.9 4.7 13.3 10.9 4 4
Mechanical stability, % 0.005 to 0.220 0.011 0.031 27.6 0.027 0.0764 67.9 4 3

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