Designation: D1417 − 16

Standard Test Methods for

Rubber Latices—Synthetic1
This standard is issued under the fixed designation D1417; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope D1418 Practice for Rubber and Rubber Latices—

1.1 These test methods cover test procedures for synthetic Nomenclature
rubber latices ABR, BR, CR, IIR, IR, NBR, NCR, NIR, PBR, D1646 Test Methods for Rubber—Viscosity, Stress
PSBR, SBR, SCR, SIR, synthetic rubber latices having substi- Relaxation, and Pre-Vulcanization Characteristics
tute carboxylic acid (COOH) groups on the polymer chain (X), (Mooney Viscometer)
and synthetic rubber latices that are reinforced (Y). Exceptions D3182 Practice for Rubber—Materials, Equipment, and Pro-
to the above are noted in the individual test procedures. The cedures for Mixing Standard Compounds and Preparing
test methods include procedures for sampling, and for deter- Standard Vulcanized Sheets
mining total solids, volatile unsaturates (residual styrene), pH D3314 Test Method for Rubber—Chemical Analysis for
value, surface tension, viscosity, coagulum, bound styrene, Polystyrene Blocks In SBR (Styrene-Butadiene Rubber)
Mooney viscosity, mechanical stability, polystyrene reinforce- and Styrene-Reinforced Latices
ment in contained polymer, and residual acrylonitrile content. D4483 Practice for Evaluating Precision for Test Method
Standards in the Rubber and Carbon Black Manufacturing
NOTE 1—The nomenclature used in these test methods is in accordance Industries
with Practice D1418.
D6204 Test Method for Rubber—Measurement of Unvulca-
1.2 The values stated in SI units are to be regarded as nized Rheological Properties Using Rotorless Shear Rhe-
standard. ometers
1.3 This standard does not purport to address all of the E70 Test Method for pH of Aqueous Solutions With the
safety concerns, if any, associated with its use. It is the Glass Electrode
responsibility of the user of this standard to establish appro- E200 Practice for Preparation, Standardization, and Storage
priate safety and health practices and determine the applica- of Standard and Reagent Solutions for Chemical Analysis
bility of regulatory limitations prior to use. E1970 Practice for Statistical Treatment of Thermoanalytical
Data
2. Referenced Documents E2975 Test Method for Calibration of Concentric Cylinder
Rotational Viscometers
2.1 ASTM Standards:2
D1076 Specification for Rubber—Concentrated, Ammonia 3. Sampling
Preserved, Creamed, and Centrifuged Natural Latex 3.1 Rubber latex tends to cream on standing. Once stratifi-
D1331 Test Methods for Surface and Interfacial Tension of cation has occurred, the latex must be thoroughly agitated to
Solutions of Paints, Solvents, Solutions of Surface-Active obtain a homogeneous blend as a representative sub-sample.
Agents, and Related Materials The procedure required differs with the type of container and
D1416 Test Methods for Rubber from Synthetic Sources— facilities available.
Chemical Analysis (Withdrawn 1996)3
3.2 Sub-Sampling from Tank Cars:
3.2.1 If stratification has occurred, take separate samples
1
about 75 mm (3 in.) from the top surface and about 75 mm
These test methods are under the jurisdiction of ASTM Committee D11 on
from the bottom of the tank. If results from the top and bottom
Rubber and are the direct responsibility of Subcommittee D11.23 on Synthetic
Rubbers. samples do not agree within 1 % total solids, the contents of the
Current edition approved June 1, 2016. Published June 2016. Originally car shall be thoroughly agitated until samples obtained do
approved in 1956. Last previous edition approved in 2010 as D1417 – 10. DOI: agree within this tolerance.
10.1520/D1417-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 3.3 Sub-Sampling from Drums:
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM 3.3.1 Blending—The latex shall be blended by one of the
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
following test methods:
3
The last approved version of this historical standard is referenced on 3.3.1.1 Test Method A—If the drum is fitted with a bung and
www.astm.org. contains at least 2 % air space, lay it on its side and roll back

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

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 D1417 − 16
TABLE 1 Drying Time for Determination of Total Solids in Latex where taken at different depths, for example from tanks, the
(Drying Aid, 1 cm3 of distilled water.) sub-samples shall be combined and thoroughly blended by
Type of Latex Drying Time, min stirring or shaking immediately before the final sample is
SBR 2000 45 taken.
SBR 2001 45
SBR 2002 45
SBR 2003 45 4. Total Solids
BR 2004 45
SBR 2005 45 4.1 Apparatus:
SBR 2006 45
SBR 2076 45 4.1.1 Tared, covered, all-metal ointment boxes, having a
SBR 2100 60 capacity of approximately 50 to 60 cm3, a minimum diameter
SBR 2101 and X765 45 of 38 mm (1.5 in.), and a maximum height of 23 mm (0.9 in.).
SBR 2102 60
SBR 2103 60 The disposable aluminum liner for the metal ointment box may
BR 2104 45 be used.
SBR 2105 45
SBR 2106 45 4.2 Procedure:
SBR 2107 45
SBR 2108 45 4.2.1 Method A—Accurately weigh a clean, dry aluminum
SBR 2109 45 foil dish. Record the weight. Measure 2 mL of sample and put
SBR 2110 45 in the aluminum foil dish. Reweigh the dish and record the
SBR 2111 45
SBR 2112 45 weight. Put the aluminum foil dish in a 170°C oven; heat for 15
SBR 2113 45 min. Remove the aluminum foil dish from the oven and let cool
SBR 2114 45 in a desiccator. Reweigh the aluminum foil dish. Record the
weight. Calculations: A = weight of dish empty; B = weight of
dish + sample; C = weight of dish + residue;
and forth briskly for not less than 10 min. Then turn the drum ~ C 2 A !~ 100!
upside down for about 15 min and repeat the rolling operation 5 % Total Solids (1)
~B 2 A!
for an additional 10 min. If the drum contains less than 2 % air
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
means of a suitable motor-driven stirrer for as long as is Slope—0.05 % ⁄ min
necessary to disperse the cream. Excessive stirring and unnec- Program—No. 1
essary exposure of the latex to air must be avoided. A suitable A1 pans—Fisher #01-913-356
Fiber paper—Fisher #01-913-318
type of stirrer consists of a collapsible two-bladed stainless
steel propeller of 11 cm minimum diameter, when fully Place a glass fiber filter circle on an aluminum pan. Open the
opened, mounted on a stainless steel shaft sufficiently long for lid of the IR-100 and center the pan (with filter) between the
the propeller to be distant about one quarter the height of the four prongs of the“ X”-shaped holder. Close the lid and press
latex from the bottom of the drum. The stirrer shall be operated the START button. When display reads “tare pan,” press the
at a minimum speed of 900 r/min. If desired, two propellers TARE button. Raise the lid and place about 3.0 g of latex in a
may be used on the same shaft, the lower one being near the circle on the filter paper. Again close the lid. Wait 10 s, then
end of the shaft. The shaft speed shall give a brisk turnover press the START button. The instrument will automatically run
without creating a vortex. The part of the equipment immersed for about 4 min then shut off. Read the percent (%) solids
in the latex must contain no copper or brass. directly from the printout paper or from the display screen.
3.3.2 Removal of Sub-Sample—After blending, take the Report the value to the nearest 0.1 %.
sample without delay. A suitable method is by slowly inserting 4.2.3 Method C—Total solids is determined using a CEM
a clean, dry, glass tube of not more than 15 mm internal microwave oven. This unit can yield accurate results in a few
diameter and open at both ends until it reaches the bottom of minutes. For detailed operating instructions, please refer to the
the container. Then close the upper end of the tube and transfer operator’s manual.
the contents to a clean, dry sample bottle. Repeat the operation 4.2.3.1 Equipment:
until sufficient latex has been obtained. (1) Moisture/Solid Analyzer (microwave oven).
NOTE 2—Alternatively, a specially constructed metal sampling tube (2) Glass fiber sample pads.
may be used, the bottom of which can be closed by remote control. Copper (3) 5 mL Disposable Pipet.
or brass must not be used in any part of its construction. 4.2.3.2 Procedure—Put the pads on the balance. Tare the
3.3.3 Sample: weight of the pads. Apply the latex sample to the pads by using
3.3.3.1 Where sub-samples are drawn from several the pipet. Spread the latex in a zig-zag pattern. Use between 1.0
containers, for example, 10 % sampling of latex in drums, or to 5.0 g of latex. Keep sample application as uniform as

2
 D1417 − 16
possible to maximize reproducibility. Press “Start” button and lift the stopper to allow the solution to enter the flask around
read the percent solids from the display. Record the result to the stopper. Shake the bottle and contents and titrate the
one decimal place. liberated iodine with 0.1 N standard sodium thiosulfate solu-
tion to a faint yellow color. Add 1 cm3 of starch indicator
NOTE 3—An alternative method for the determination of total solids in
synthetic rubber latex is described in Specification D1076. solution and continue the titration with sodium thiosulfate
solution until the solution is clear.
5. Volatile Unsaturates (Residual Styrene) 5.4.3.1 For a blank determination, repeat the procedure
using distilled water instead of latex.
5.1 Scope—This test method measures the residual styrene
of SBR synthetic rubber latices. It is not applicable to other 5.5 Calculation—Calculate the percentage of volatile un-
synthetic rubber latices. saturates (residual styrene) as follows:
5.2 Apparatus: Volatile unsaturates ~ residual styrene! , % (2)
5.2.1 Iodine flasks having capacities of 250 cm3 each, and
5 $ @ ~ D 3 E ! 2 ~ F 3 G ! # 3 0.0521 3 100/M % 2 H
distillation apparatus with ground-glass joints.
5.2.2 25-cm3 pipet. where:
5.2.3 50-cm3 buret. D = cubic centimetres of standard bromide-bromate solu-
5.3 Reagents: tion used,
5.3.1 Synthetic Methanol, containing 100 ppm of p-tertiary E = normality of the bromide-bromate solution,
butyl catechol. F = cubic centimetres of standard thiosulfate solution used
for the titration,
5.3.2 Standard Potassium Bromide-Potassium Bromate So-
G = normality of the thiosulfate solution,
lution (0.1 N)—Dissolve 2.784 g of potassium bromate H = blank determination, %, and
(KBrO3) and 10.0 g of potassium bromide (KBr) in water and M = mass of latex used, g.
dilute to 1000 cm3. Standardize with 0.1 N sodium thiosulfate
(Na2S2O3) solution in the presence of an excess (about 3 g) of 6. pH Value
potassium iodide (KI) and sulfuric acid (H2SO4), (18 %).
5.3.3 Sulfuric Acid Solution (18 %). 6.1 Apparatus—Any pH electrometer and a glass electrode-
5.3.4 Potassium Iodide Solution (10 %). calomel cell assembly may be used as described in Test
5.3.5 Standard Sodium Thiosulfate Solution (0.1 N). Method E70. A flowing calomel electrode has been found
5.3.6 Starch Indicator Solution. 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 Procedure:
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 6.3 Procedure—Before making a determination take care
butyl catechol. Be sure to add the materials in the following that the instrument is properly standardized at frequent inter-
order: 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
bottle to stand for 60 s. If no yellow color remains, add 7.2 Apparatus—Use a du Nouy tensiometer, carefully cali-
successive 10-cm3 portions of the bromide-bromate solution brated as described in Test Methods D1331.
until a slight yellow color persists for 60 s after the addition. 7.3 Procedure—Strain approximately 25 cm3 of latex, ad-
Make the additions by drawing the standard solution from the justed to a temperature of 25 6 2°C, into a pan 60 to 65 mm
buret into the funnel lip and lifting the stopper so that the (2.4 to 2.6 in.) in diameter and 18 to 20 mm (0.7 to 0.8 in.) high
solution enters the flask around the stopper. Wash the funnel lip (Note 4). The surface of the latex must be free of air bubbles,
with distilled water in the same manner and seal with water. and the surface tension test shall be within 3 to 4 min to avoid“
After 60 s has elapsed since the final bromide-bromate skinning over” of the latex. Clean the tensiometer ring by
addition, add 10 cm3 of 10 % KI solution to the funnel lip, and heating in a bunsen flame. Extreme care must be taken to avoid

3
 D1417 − 16
distortion as the tensiometer ring is handled. Place the pan, 8.3.4.1 Drive Motor, to apply a rotational displacement to
containing the latex being tested, beneath the ring on the the specimen at a rate of 0.6 r/min to 60 r/min constant to 6 1
adjustable platform of the instrument. With the instrument % full scale,
adjusted so that the ring system is in its zero position when the 8.3.4.2 Coupling Shaft, or other means to transmit the
ring is dry and the scale reading is zero, raise the platform until rotational displacement form the motor to the specimen,
the latex makes contact with the ring. Submerge the ring 8.3.4.3 Spindle, suitable for the viscosity range from 6
beneath the surface of the latex. Now slowly lower the mPa·s to 40 mPa·s to fix the specimen between the drive shaft
platform by means of the platform-adjusting screw and in- and a stationary position,
crease the torsion of the wire simultaneously, proportioning 8.3.4.4 Sensor, to measure the torque developed by the
these two adjustments so that the torsion arm remains exactly specimen to within 6 1 % full scale,
in its zero position. As the film adhering to the ring approaches 8.3.4.5 Data Collection Device, to provide a means for
the breaking point, proceed more slowly with the adjustments acquiring, torque, rotational speed, temperature and time.
to make certain that the moving system is in its zero position 8.3.4.6 Guard, to protect the spindle from mechanical dam-
when the rupture occurs. The scale reading at which the ring age.
detaches from the latex represents, after proper correction, the 8.3.4.7 Data Collection Device, to provide a means of
surface tension of the latex at the given temperature. Record acquiring, storing, and displaying measured or calculated
the average of three consecutive readings, discounting the first signals, or both. The minimum output signals required for
reading. The ring is cleaned by flaming between readings and rotational viscosity are torque, rotational speed, temperature
all readings shall agree within 0.5 mN/m (0.5 dynes/cm). and time.
NOTE 4—The pan must be free of an oil film since traces of oil 8.3.4.8 Specimen Container, of approximately 240 mL (8-
introduce variable results in the surface tension measurement. oz) capacity to contain the test specimen during testing.
7.4 Calculations—Calculate the surface tension, in 8.3.4.9 Stand, to support, level, and adjust the height of the
millinewtons/meter (dynes, per centimeter), as follows: drive motor, shaft and spindle.
8.3.4.10 Level, to indicate the vertical plumb of the drive
Surface tension, mN/m 5 M 3 N (3)
motor, shaft and spindle.
where: 8.3.4.11 Auxiliary instrumentation considered necessary or
M = reading of the tensiometer, and useful in conducting this method includes:
N = a correction factor calculated as follows: (1) Data analysis capability to provide viscosity, stress or
other useful parameters derived from measured signals.
N 5 0.72501 =@ ~ 0.0003678 3 M ! /R 2 # 1P (4) 8.3.5 Temperture Sensor, to provide an indication of the
where: specimen temperature of the range of 20°C to 30°C to within
M = reading of the tensiometer, 6 0.1°C.
R = radius of the ring, cm, and 8.4 Preparation of Sample:
P = a constant calculated as follows: 8.4.1 If the latex contains occluded air, remove the air in the
P 5 0.04534 2 ~ 1.679S/R ! (5) following manner before proceeding with the determination of
viscosity. After diluting the latex (if viscosity is to be deter-
where:
mined at lower designated solids) with distilled water to the
S = radius of the wire of the ring, cm, and approximate desired total solids, pour a sufficient volume of
R = radius of the ring, cm. the latex into a three-necked distillation flask equipped with a
stirrer and vacuum connections so that at least 500 cm3 of latex
8. Viscosity will remain after the removal of the air.
8.1 Scope—This test method covers the determination of the 8.4.2 Start the agitator and evacuate the flask to 3.4 to 3.8
viscosity of synthetic rubber latices using a rotational viscom- kPa (approximately 1 in. Hg) or until the foam rises into the
eter. neck of the flask. Break the vacuum. Evacuate several times in
this manner to ensure removal of the occluded air.
8.2 Summary of Test Method—The viscosity is determined
8.4.3 Strain the deaerated latex through a 355-µm standard
by means of a rotational viscometer that measures the torque
screen. Determine the total solids content of the latex and then
produced on a specified spindle rotating at constant speed
accurately adjust the solids content of the latex to the desig-
while immersed to a given depth in the latex.
nated total solids content by the addition of distilled water. Add
8.3 Apparatus: the water slowly to the latex, and gently stir the mixture with
8.3.1 Glass Stirring Rod. a glass rod during the dilution.
8.3.2 Screen—Standard sieve 355 µm. 8.5 Procedure:
8.3.3 Distillation Flask, three-necked, equipped with a stir- 8.5.1 Perform any viscometer calibration procedures de-
rer and vacuum connections. scribed by the apparatus manufacturer in the operations
8.3.4 Rotational Viscometer—The essential instrumentation manual. (See Test Method E2975.)
required providing the minimum rotational viscometer analyti- 8.5.2 From an estimation of the viscosity of the test speci-
cal capability for this method include: men (nominally 6 mPa·s to 40 mPa·s), select a spindle and

4
 D1417 − 16
rotational speed that will produce readings nearest the midpoint ~ Weight of filter & residue! 2 ~ Weight of filter! x 1 000
of the measurable viscosity scale. 5 Residue, in ppm (8)
8.5.2.1 The viscometer scale reading shall be within the NOTE 8—When mechanically concentrated latices are tested, use
range of 10 to 95 % of full scale. distilled water as the diluent.
8.5.3 Measure the temperature of the strained latex and
ensure that it is within the range of 23 to 27°C. 10. Determination of Bound Styrene in Contained
8.5.4 Pour approximately 200 mL of latex into the 240 mL Polymer
container. 10.1 Scope—This test method is designed to measure the
8.5.5 Lower the viscometer (or raise the container) until the bound styrene content of butadiene-styrene copolymers. The
height of the latex is at the indicated level on the spindle. test method is not applicable when a high styrene latex (above
50 % bound styrene) is a component of the latex system.
NOTE 5—Holding the container at an angle helps to prevent air bubbles
from being trapped under the spindle during loading. 10.2 Coagulation Procedure—Use the test method outlined
8.5.6 Initiate the rotation of the spindle at the rotational in 11.5.
speed selected in step 8.5.2. 10.3 Bound Styrene Determination—Use the test method
8.5.7 After 60 s measure the viscosity (η(1) (or torque (τ(1) described in Test Methods D1416.
and rotational velocity (ώ(1)) as described by the apparatus
manufacturer in the operations manual. 11. Determination of Mooney Viscosity or Rotorless
8.5.8 Repeat 8.5.7 two additional times to obtain η(2) and Shear Rheometer Rheological Properteis of
η(3) or τ(2), τ(3), ώ(2) and ώ(3). Contained Polymer
8.5.9 Calculate and report the mean viscosity (η) in mPa·s 11.1 Scope—This test method is designed to measure the
(cP) (see Practice E1970). viscosity and rheological properties of the contained polymer
NOTE 6—If it is desired to better characterize the latex, additional of anionic stabilized synthetic rubber latices having a residual
rotational speeds may be used. monomer content of less than 0.50 % by weight. It is not
applicable to latices of polymers containing substitute carbox-
9. Coagulum Content
ylic acid groups on the polymer chain, hot polymerized BR
9.1 Apparatus: (2004), CR, NCR, SCR, or ABR.
9.1.1 Nylon filter cloth, 25 micron.
11.2 Summary of Test Method—The latex is coagulated by
9.1.2 Beaker, tared.
the consecutive addition of salt, methanol, and acid solutions
9.1.3 Demineralized Water (DMW).
while under fast agitation. The resulting crumb is filtered,
9.1.4 Air Oven.
dried, and massed on a rubber mill. The viscosity of the
9.1.5 Desiccator.
contained polymer is measured in a shearing disk viscometer.
9.2 Procedure—Store clean nylon (25 micron mesh) filter
11.3 Apparatus:
circles (9.0 6 0.2 cm in diameter) in a desiccator. Weigh the
11.3.1 Blendor4—Explosion-proof type.
clean filter and record this weight to four decimal places. Place
11.3.2 Cheesecloth.
the filter on the porcelain Buchner funnel; set the funnel on a
11.3.3 Drying Tray, approximately 30 by 20 by 2.5 cm (12
2000-mL flask. Weigh 500 6 0.5 g of latex sample into a
by 8 by 1 in.) with a 1.00 to 1.41 mm mesh plastic screen
1200-mL beaker. Add 500 6 1 mL of DMW and stir gently.
supported by a coarse screen bottom.
Filter the sample through the nylon filter with the aspirator
11.3.4 Draft Oven, maintained at 125 6 2°C.
slowly. If drainage stops, use a plastic pipet and gently swirl
11.3.5 Laboratory Mill, as described in Practice D3182.
the liquid in a whirlpool fashion slowly, taking care not to
11.3.6 Shearing Disk Viscometer, as described in Test Meth-
touch the nylon filter on the bottom of the liquid. This usually
ods D1646, or Rotorless Shear Rheometer, as described in Test
allows drainage to resume. Rinse the filter gently with squirts
Method D6204.
of DMW (50 mL). All latex must be rinsed through the filter.
Dry the filters in the 70°C blue M oven for 15 min. 11.4 Reagents and Materials:
11.4.1 Sodium Chloride Solution (250 g/dm3)—Dissolve
NOTE 7—Take care not to lose any floc in transferring from oven to
counter to balances. Cool the filter for 15 min in a desiccator. Weigh the
250 g of ACS Grade NaCl in 1 dm3 of demineralized water.
filter plus residue to four (4) decimal places. Calculate and report the 11.4.2 Methanol Solution (7.5 g/dm3)—Dissolve 7.5 g of a
residue to the nearest third decimal place [Spec:0.010 % maximum]. suitable antioxidant5 in 1 dm3 of USP methanol.
9.3 Calculation: 11.4.3 Sulfuric Acid (1 + 9)—Add 100 cm3 of concentrated
ACS Grade H2SO4 (sp gr 1.84) to 900 cm3 of demineralized
~ Weight of filter& residue! 2 ~ Weight of filter! water.
5 % Residue (6)
5 11.4.4 Congo Red Indicator Paper.
For a 500 gram sample:
~ Weight of filter & residue! 2 ~ Weight of filter! 4
A Model FCI-15 Waring Blendor, or equivalent, has been found satisfactory for
5 % Residue (7)
5 this purpose.
5
Antioxidants of the bis or polyphenol types such as Ethyl 702, Santowhite
9.3.1 Alternate Calculation: The residue may also be ex- Powder, and Wingstay L, and of the diaryl-p-phenylenediamine type such as
pressed in terms of parts per million (ppm), as follows: Wingstay 200, have been found to be equivalent to PBNA.

5
 D1417 − 16
11.4.5 Agerite White (KD-64 Harwick) stock dispersion temperature at 8565°F and the distance between rolls at
11.4.6 2.2 % Aluminum Sulfate, dissolve 378 grams in 5 0.06560.005 inches. With the speed set at 40 rpm, pass the
gallons of tap water and agitate vigorously. Some precipitate sample through the mill ten times, doubling it during passes 2
will remain in the reagent. through 9. Do not band the material, or let it stick to the rolls
11.5 Procedure: so that it is carried around. It may be necessary to actually stop
the mill after each pass in order to make seperate, independent
11.5.1 Coagulation Procedure—If the total solids content of
passes. Allow the milled samples to sit for thirty minutes at
the latex is greater than 30 %, dilute the latex with distilled
room temperature before testing.
water to a total solids contents of approximately 30 %. Add to
11.5.4.4 Determination of Mooney Viscosity—After the
250 cm3 of the diluted latex, 50 cm3 of the NaCl solution and
sample has been prepared as detailed above, run the Mooney
mix thoroughly.
test as listed in Test Methods D1646, Paragraphs 9–12.
11.5.1.1 Add 250 cm3 of methanol-anti-oxidant solution
while continuing to agitate. Add 10 cm3 of H2SO4 (1 + 9) 12. Determination of Mechanical Stability
slowly during a period of 2 to 3 min. If the coagulating solution 12.1 Scope—This test method covers the determination of
does not turn Congo Red paper from red to blue, add additional the stability of synthetic latices when subjected to highspeed
H2SO4 while stirring until the color does change. mechanical stirring.
11.5.1.2 Pour the contents of the coagulating cup onto
cheesecloth and press as much serum as possible from the 12.2 Summary of Test Method—A sample of latex is sub-
mass. Hand separate the mass, wash it thoroughly with jected to mechanical shear by the use of a high-speed stirrer
demineralized water, and transfer the pieces to a drying tray. and the extent of instability noted. The amount of coagulum
11.5.2 Drying Procedure—Dry the crumb in a draft oven at formed after a given time of agitation is considered a measure
125 6 2°C. Drying time will vary with the crumb consistency, of latex instability.
polymer viscosity, and oven conditions and should be deter- 12.3 Apparatus:
mined by experimentation. Drying time shall be determined by 12.3.1 Tester6—The test apparatus shall consist of a vertical
reference to a volatile matter versus time plot. The desired shaft high-speed stirrer capable of maintaining a speed of
drying time shall be taken at a time less than 5 min after the 14 0006 200 r/min for the duration of the test. The stirrer shaft
minimum level has been reached. Over drying and under shall be approximately 6.3 mm (0.25 in.) in diameter at its
drying will both give incorrect Mooney viscosity values and lower end at the point of attachment of the agitator disk and
are to be avoided. may taper upward for greater strength. It shall be of sufficient
11.5.3 Determination of Mooney Viscosity or Processability length to reach conveniently to the bottom of the test bottle.
Characteristics—Mill mass the rubber and determine the The shaft shall run with not more than 0.25 mm (0.010 in.) out
Mooney viscosity in accordance with Test Methods D1646, or of true at the speed specified.
processability characteristics in accordance with Test Methods 12.3.2 Agitator Disk—The agitator itself shall consist of a
D6204. polished stainless steel disk 36.12 6 0.03 mm (1.4226 0.001
11.5.4 Special Procedure for Vinylpyridine latex (PSBR): in.) in diameter and 1.58 6 0.05 mm (0.062 6 0.002 in.) in
11.5.4.1 Coagulation of Latex—Add 2400 ml of warm water thickness having a threaded stud at its exact center for
(130°F) to the container and start agitation. Add 25 ml of attachment to the center of the lower end of the stirrer shaft.
Agerite White Dispersion. Add 200 ml of latex to be tested (or 12.3.3 Test Bottle—The test bottle shall be a flat-bottom
sufficient to provide 75–80 grams of polymer). Increase agita- cylindrical glass container 57.8 6 1 mm (2.28 6 0.04 in.) in
tion and slowly add 2 % aluminum sulfate (increase agitation if inside diameter by approximately 12.7 cm (5 in.) in height, and
coagulated polymer starts to form a ball) until coagulation is having a wall thickness of approximately 2.3 mm (0.09 in.).
complete. This can be determined by observing the serum. The 12.3.4 Bottle Holder—The bottle holder shall be so con-
serum solution will be relatively clear and contain a few very structed that the bottle may be conveniently lowered and raised
fine particles when coagulation is complete. Continue agitation to the exact specified position with relation to the shaft and
for one (1) minute after complete coagulation. Allow to stand agitator. The position of the test bottle shall be such that the
for 10 minutes. Seperate the crumb from the serum by filtering axis of the stirrer shaft is concentric with the axis of the bottle
through a fine, lint-free cloth. and that the bottom of the agitator disk is 12.7 6 2 mm (0.5 6
11.5.4.2 Drying—The coagulum during filtration may tend 0.1 in.) from the bottom inside of the bottle.
to agglomerate into a mass. Break this mass into very small 12.3.5 Stainless Steel Screen—No. 180 µm sieve with 0.180
pieces. Dry the crumb in an air oven at 90°C. When the crumb 6 0.009-mm (0.0070 6 0.0004-in.) opening and 0.131 6
is dry, it will completely lose its white color and turn brown. 0.01-mm (0.0052 6 0.0005-in.) wire diameter. The screen
This should require 11⁄2 to 21⁄2 hours. Check for dryness after shall be cut to fit into the seat of a pipe union having inside
one (1) hour drying time and every 15 minutes thereafter til diameter of about 5 cm (nominal 11⁄2-in. pipe size).
dry. Remove when dry. To determine if the crumb is dry, pull 12.4 Procedure:
several pieces apart and, if any white shows, dry for an 12.4.1 If the viscosity of the latex as determined by Section
additional 1⁄2 hour. Do this until the crumb is completely dry. 8 of this test method is greater than 350 mPa·s (cP), dilute the
11.5.4.3 Milling of Crumb—Using the sample prepared in
10.4.2 above, mass the crumb together into a ball in your 6
The sole source of supply of the apparatus known to the committee at this time
hands. Ensure that the dry crumb is at least 60 grams. Set mill is Custom Scientific Instruments, Inc., 13 Wing Dr., Whippany, NJ 07981.

6
 D1417 − 16
latex with sufficient water so that the viscosity is below 350 screen. Wash the residue from the cup through the screen using
mPa·s (cP), except that in no case should the latex solids be additional wash water. Dry to constant weight using micro-
reduced by more than 10 % relative. wave oven. Reweigh the screen containing the dried coagulum
12.4.2 Strain the latex through a 180-µm sieve and weigh 50 and find by difference the amount of coagulum collected.
6 0.5 g of the strained latex into the test bottle. Place the bottle Express the final results in ppm as shown below:
containing the latex in the holder of the stability tester. Grams Coagulum
12.4.3 Start the tester and agitate for exactly 30 min (or 3 1,000,000 5 ppm Residue (11)
150
other agreed-upon time) at 1470 6 21 rad/s (14 000 6 200
r/min). The time of agitation should be adjusted so that the 12.8 Centrifuge Stability
temperature of the latex does not increase to more than 60°C. 12.8.1 Scope—This method was designed to readily predict
Remove the sample immediately to avoid any filming and rinse creaming stability of vinylpyridine containing latices. The
the agitator shaft and disk with distilled water. Strain the latex amount of agglomerated cream is determined after diliting,
through a tared 180-µm screen that has previously been wetted centrifuging and filtering.
with a 2 % aqueous solution of a surfactant such as potassium 12.8.2 Equipment:
oleate. Finally, flush the screen with the same solution and then (1) Centrifuge, Sorvall GLC1 or equivalent, at least 2500
follow with a rinse of distilled water. Dry the screen and rpm
coagulum in a force draft oven at 100 6 2°C to constant mass (2) Centrifuge jars, 100 mL with caps
(approximately 15 min). Cool and weigh again to 60.001 g. (3) Jars, 1 qt, wide mouth, with lids
(4) Balance, 3000 g capacity
12.5 Calculation—Calculate the percent coagulum as fol- (5) Balance, Analytical 6 0.1 mg
lows: (6) Screen, 325 mesh, to fit residue holders
Coagulum, % 5 @ ~ A 2 B ! /50# 3 100 (9) 12.8.3 Procedure:
12.8.3.1 Mix the latex well and filter through a paint
where: strainer. Dilute the amount of latex obtained from from the
A = mass of tared screen plus coagulum, and formula listed in 13.4.1 below to 900 grams with deionized
B = mass of tared screen. water and mix well. Immediately transfer 100 ml of the diluted
12.5.1 Alternate Calculation—The coagulum may also be latex to a 100 ml centrifuge jar. Make certain that the jar is
expressed in terms of parts per million (ppm), as follows: clean and dry. Centrifuge the 100 ml sample at 2200 rpm for 1
Coagulum, ppm 5 @ ~ A 2 B ! /50# x 1 000 000 (10)
hour. After centrifuging, pour the liquid through a tared 325
mesh screen. Rinse the jar several times, pouring each rinse
12.6 Report—Report the percent coagulum, the total solids through the filter. Dry the screen in a microwave over for 3
content at which the latex was tested, and the duration of minutes on high and weigh. Record the weight of residue as
stirring, in minutes. specified by the calculation listed in 3.4.2 below.
12.7 Mechanical Stability of Latex (Alternate method) 12.8.4 Calculations:
12.7.1 Scope—This method determines the amount of latex 900 3 30
which is coagulated under shearing conditions of the test. A Grams of latex to dilute 5 (12)
TSC
sample of latex is subjected to mechanical shear by the use of
Grams of residue 3 10,000 ppm 5 residue in ppm (13)
a high speed stirrer and the extent of instability is noted. The
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:
(1) 200 mesh screen 13.1 Scope—This test method is designed to measure the
(2) 80 mesh polyester screen polystyrene content of polystyrene-reinforced SBR latices in
(3) 100 mL graduated cylinder the range from 1 to 100 % polystyrene. The test method is not
(4) Hamilton Beach Drinkmaster No. 30 applicable on polymers containing gel, unless it has been
(5) Plastic seal for the mixer cup (1 qt) proven that gel does not interfere.
(6) Clamp, screw chain 13.2 Procedure—Determine the polystyrene content in ac-
(7) Microwave oven cordance with Test Method D3314.
12.7.3 Procedure—Cool the latex to 100°F if it is found to
be above this temperature. Filter approximately 170 ml of latex 14. Determination of Residual Acrylonitrile Content
through a 200 mesh screen. Pour 150 ml of this latex into the 14.1 Scope—This test method measures the residual acry-
mixer cup. To eliminate air drying, place the plastic seal over lonitrile content of nitrile rubber latices that have a residual
the mixer cup and secure with the chain clamp while the test is acrylonitrile content of less than 0.2 %.
running. Agitate on the Hamilton Beach mixer for 30 minutes
at the “low” setting. Preweigh an 80 mesh polyester screen. At 14.2 Summary of Test Method—The latex is distilled and the
the conclusion of the test, inspect the sample for air dried latex. distillate is collected in methanol. n-Dodecyl mercaptan is
If any is found, dispose of the sample and rerun, making sure added to the distillate and the excess is titrated with iodine
that the seal is tight. Immediately after removing the mixer cup, solution.
pour the latex through the preweighed 80 mesh polyester 14.3 Apparatus:

7
 D1417 − 16
14.3.1 Distillation Apparatus, consisting of a 500-cm3 dis- 14.5.1 Weigh 25.0 6 0.2 g of latex into the distillation flask
tillation flask, still head, vertical water-cooled condenser, and and add 100 cm3 of water and 1 cm3 of a suitable silicone
100-cm3 receiver with glass stopper through which pass a glass antifoam agent. Place 25 cm3 of methanol in the receiver and
tube connected to the condenser and a shorter exit glass tube approximately 10 cm3 of methanol in the 50-cm3 beaker.
leading into a 50-cm3 beaker. Assemble the distillation apparatus so that the end of the tube
14.3.2 Volumetric Flask, 100-cm3. connected to the condenser is immersed in the methanol in the
14.3.3 Conical Flask, at least 250-cm3. receiver and the end of the exit tube connected to the receiver
14.4 Reagents: is immersed in the methanol in the 50-cm3 beaker. (The
14.4.1 Purity of Reagents—Reagent grade chemicals shall purpose of the 50-cm3 beaker is to recover any distillate not
be used in all tests. Unless otherwise indicated, it is intended collected in the receiver.) Immerse the receiver and 50-cm3
that all reagents shall conform to the specifications of the beaker in ice.
Committee on Analytical Reagents of the American Chemical 14.5.2 Distill the mixture, adjusting the rate of boiling to
Society, where such specifications are available.7 Other grades control frothing, and collect 50 cm3 of distillate in the receiver.
may be used, provided it is first ascertained that the reagent is 14.5.3 Empty the contents of the receiver and 50-cm3
of sufficiently high purity to permit its use without lessening beaker into the 100-cm3 volumetric flask. Rinse twice with
the accuracy of the determination. about 5 cm3 of methanol by pouring the methanol through the
14.4.2 Purity of Water—Unless otherwise indicated, refer- condenser into the receiver and add the washings to the
ences to water shall be understood to mean distilled water or volumetric flask. Dilute to the mark with methanol.
water of equal purity. 14.5.4 Pipet a 50-cm3 aliquot of the diluted distillate into the
14.4.3 Acetic Acid, glacial (CH3COOH). conical flask that contains 25 cm3 of 2-propanol. Pipet 10 cm3
14.4.4 n-Dodecyl Mercaptan, Alcoholic Solution(1.25 %)— of mercaptan solution into the flask. Add 1 cm3 of alcoholic
Dissolve 12.5 g of n-dodecyl mercaptan (CH3(CH2)11SH) in potassium hydroxide and allow the solution to react for exactly
500 cm3 of 2-propanol dilute to 1000 cm3. 2 min at 23 6 2°C. Add 2 cm3 of glacial acetic acid to stop the
14.4.5 Iodine Solution (0.0125 M)—Transfer 3.2 g of iodine reaction. The resulting pH value should be between 4 and 6.
and 15 g of potassium iodide (KI) to an 800-cm3 beaker, add 30 Titrate with freshly standardized iodine solution to a yellow
ml of water, and stir until all solution is complete. Dilute with color that persists for at least 60 s. Discard the iodine solution
water to 500 cm3, and filter through a sintered-glass filter. Wash remaining in the buret, unless it is required for immediate use.
the filter with about 15 cm3 of water, transfer the combined 14.5.5 Run a blank determination, omitting the distillation
filtrate and washing to a 1000-cm3 volumetric flask, dilute to stage, using 50 cm3 of 50-50 methanol-water mixture.
the mark with water, and mix. Store the solution in a glass- 14.6 Expression of Results—Calculate the residual acrylo-
stoppered, amber-glass bottle in a cool place. Standardize with nitrile content as a percentage by mass of the latex as follows:
sodium thiosulfate. A 3 ~B 2 C! 3 V 3 E 3 F
14.4.6 Methanol (CH3OH). D 3M
3 100 (14)
14.4.7 Potassium Hydroxide, Alcoholic Solution (6 %)—
Grind 6 g of potassium hydroxide (KOH) with successive which simplifies to:
25-cm3 portions of 95 % ethanol until dissolution is complete. A 3 ~ B 2 C ! 3 0.424
Dilute to 100 cm3 with 95 % ethanol. Filter immediately into a Residual acrylonitrile, % 5
D
3 100 (15)
dark bottle and keep tightly closed. Let this solution stand
overnight before using. When it becomes noticeably where:
discolored, it should be discarded. Storing in a nitrogen A = molarity of the iodine solution,
atmosphere will preserve the solution considerably. B = iodine solution used in the blank determination, cm3,
14.4.8 2-Propanol ((CH3)2CHOH). C = iodine solution used in the sample titration, cm3,
14.4.9 Sodium Carbonate (Na2CO3). D = aliquot of dilute distillate, cm3,
14.4.10 Sodium Thiosulfate Solution (0.0125 M)—Dissolve E = 2 milliequivalents of iodine per millimole of iodine,
F = 0.05306 of acrylonitrile per millimole,
3.1 g of sodium thiosulfate (Na2S2O3·5H2O) in 500 cm3 of
M = mass of sample, 25 g, and
freshly boiled and cooled water, and add 0.1 g of sodium V = total volume of distillate, 100 cm3.
carbonate (Na2CO3). Dilute to 1000 cm3 with freshly boiled
and cooled water, and let stand for 24 h. Store the solution in The results of duplicate determinations shall agree within
a tightly closed glass bottle. Standardize in accordance with the 0.005 % absolute.
procedure in Practice E200.
14.4.11 Silicone Antifoam Agent. 15. Particle Size Determination
14.5 Procedure: 15.1 Apparatus:
15.1.1 Malvern Autosizer:
15.2 Procedure:
7
Reagent Chemicals, American Chemical Society Specifications, Am. Chemical 15.2.1 Turn on Malvern Autosizer 2c for warm-up. Warm
Soc., Washington, DC. For suggestions on the testing of reagents not listed by the
up for two minutes. Select option nine from starting menu
American Chemical Society, see Reagent Chemicals and Standards, by Joseph
Rosin, D. Van Nostrand Co., Inc., New York, NY, and the United States Pharma- program on computer. Make sure temperature on Malvern is
copeia. 25°C or 60.2. Adjust if needed. Make sure beam size on

8
 D1417 − 16
Malvern is set to small. Select F2 for sample description; the crystals with Tetrahydrofuran solvent. Repeat the procedure
follow screen instructions. Toggle F5 key for results printout two more times, so that triplicate analyses are obtained.
option. 16.4 Calibration:
15.3 Preparation of Sample: 16.4.1 Obtain styrene-butadiene-vinylpyridine latices where
15.3.1 Using a 5-mL syringe, filter 20 mL DMW into a the bound monomers are accurately known. At least two
clean 50-mL beaker using a corning disposable sterile syringe different levels of vinylpyridine are needed. The following
filter. Also with the syringe, filter DMW into a four-sided relationships are used for the calibrations:
cuvette to 2⁄3 full capacity. Using a disposable pipette, add one C styrene A 1490
drop of latex to the 50-mL beaker. Swirl beaker until solution 5 a1b (16)
C VP A 1470
is uniform. Using a disposable pipette, transfer three drops of
C styrene A 1490
solution into the cuvette. Cover top with a small piece of 5 g1h (17)
C BD A 910
parafilm and shake for a few seconds. Remove parafilm and
insert a plastic cuvette top snugly. Place sample in Branson C styrene1C VP1C BD 5 100 (18)
1200 ultrasonic cleaner and sonicate for 30 s. Remove sample where:
and dry outside of cuvette with a Kimwipe. Place cuvette into Cx = wt. % values for the given monomer
autosizer machine and close door (beam size—SMALL). Ax = absorbance at wavelength X
15.4 Analysis of Sample: Constants a, b, g and h are then determined from a series of
15.4.1 Adjust counts/1000 using the dial on top of the standard latices containing different known levels of the
autosizer. Adjust to approximately 100. Sample level should be monomers. Concentration values for vinylpyridine can also be
near “ideal.” If not, adjust very gently with beam dial (near obtained by determining total nitrogen content using the
150) or dilute the latex sample. If printout is desired, make sure Kjeldahl or Dumas procedures (preferably the latter).
printer ribbon is even with top of page. Printer: Power, ready, However, to use the total nitrogen methods requires that no
and on-line lights should be illuminated. F4 key starts sample other nitrogen containing compounds be present.
measurement. Printout starts after about 4.5 min. Printing lasts
16.5 Calculation:
for approximately 1 min. The Z average mean value at the end
16.5.1 After the four constants listed above (a, b, g and h )
of the printout is recorded as particle size. Space key returns
are determined, the three equations listed in 5.4.1 above can
user to menu screen. E exits program. Turn off Malvern
then be solved simultaneously. A computer program can be set
instrument.
up to perform these calculations.
16. Bound Monomers in Vinylpyridine Latex
17. Residual Monomers
16.1 Scope—This test method covers the range of 17.1 Scope—This method describes the operation of the
vinylpyridine, styrene and butadiene normally encountered Perkin Elmer gas chromatograph. This instrument is used to
with vinylpyridine containing latices. It is not applicable to test for residual monomers in the latex, as well as the purity of
other synthetic latices. This method utilizes the infrared ab- the raw material. The use of the sample encapsulating unit is
sorption bands at 1490, 1470 and 910 cm –1 wavenumbers described. The method can be applied to any liquid sample and
arising from C = C stretching modes in styrene and vinylpyri- many solis samples provided the proper columns and condi-
dine and CH=CH2 bending of the vinyl groups of polybutadi- tions are used. This preferred method is Test Method D4026 –
ene segments, respectively. Because only absorption ratios are Method B. This method may not give the same results as the
used in the calculations, the need to determine film thickness is wet method.
eliminated.
17.2 Equipment: 1. Perkin Elmer gas chromatograph,
16.2 Apparatus: Model 3920 or Sigma 2, with FID
16.2.1 Double beam infrared spectrophotometer, Model 283 2. Column P&E10 % apiezon L on 80/100 chromosorb W, or
or equivalent. Supelco 10 % SP 2100 and 80/100 Supelcoport.
16.2.2 KRS-5 crystals - 25 × 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
7. Micropipettes, for Micropipetter above, 1 µl, Fisher No.
16.3.1 Place a drop or two of latex on a KRS-5 crystal.
21-170-11
Spread the latex evenly over the entire crystal as quickly as
8. Absorbent tissues, Kimwipes, or equivalent
possible with an applicator stick. Allow to dry under a heat
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 13. Analytical balance
wavelength regions 1550–1450 cm−1 and 950–850 cm−1. Clean 17.3 Reagents:

9
 D1417 − 16

1. Gases: –Helium, the regulator outlet pressure should be set at 70 psig. sample into the instrument, just short of puncturing the capsule.
–Hydrogen, the regulator outlet pressure should be set at 20 psig. The capsule should be in the injection port section to be heated.
– Plant air, the regulator outlet pressure should be set at 35 psig
on No.1 and 2 (Model 3920) and No. 3 (Sigma 2) instruments. All
After 15 s, insert the capsule holder all the way into the
gases must be of prepure quality. instrument to puncture the capsule. The forepart of the capsule
2. Volatile Standard, 99.9 % purity holder will be almost flush with the front of the instrument.
a. Butadiene
b. 4-Vinylcylcohexane Immediately after injecting the sample, press the start button
c. Ethlybenzene on the instrument. This starts the instrument and the computer.
d. Styrene At the end of the cycle, the oven will cool and the results will
e. Vinylpyridine
f. Other monomers and solvents as requested be printed out. When the instrument has cooled to the initial
3. Control latex with known level of styrene. temperature, another sample can be injected.
4. Solvent, carbon disulfide (CS2), chromatographic grade.
5. Methyl alcohol, chromatographic grade
17.4.3 Preparation of Standards for Instrument Standard-
ization:
17.4 Procedure:
17.4.3.1 Liquid Monomers (Styrene, VP, etc): Place 100 ml
17.4.1 Capsulating the Sample:
of carbon bisulfide in the pressure bottle and seal tightly.
17.4.1.1 Using forceps, transfer a capsule to a 10 capsule
Transfer approximately 2 ml of monomer into a Pressure-Lok
magazine. The capsule must fit securely. Use new plastic
syringe and close the valve. Expel any air. Make certain the
magazine inserts if the capsule is not held securely. Using a No.
syringe does not leak. Using an absorbent tissue, clean the
1 cork bore, cut out a piece of filter paper and insert in the
outside of the syringe and weigh. Carefully inject the required
bottom of the capsule. Place the capsule magazine in the
amount of monomer into the pressure bottle below the liquid
sealing unit with the capsule opposite the cutting blade.
surface and mix. Withdraw the syringe and re-weigh. Follow
Loosening the knurled knob on the micropipettor, carefully
the above procedure for each addition of monomer. The
insert a micropipette and tighten the knurled knob securely.
syringe may have to be refilled. Any excess monomer should
Depress the plunger and insert the pipette into the sample. With
be expelled into a solvent waste safety can for proper disposal
the pipette still in the sample, release the plunger. The sample
and the syringe should be rinsed copiously with methyl alcohol
will be in the micropipette. Remove the pipette from the
and allowed to air dry.
sample. Wipe the outside of the pipette with a tissue. Discharge
it into the capsule, touching the filter paper. Quickly seal the 17.4.3.2 Butadiene (Bd): Obtain a small sample of butadi-
capsule by pulling down on the crimping lever. The sealed ene (liquid) and place it on dry ice. Place a 2 ml Pressure-Lok
capsule in the magazine is then transferred to the capsule syringe in the freezer and allow it to come to freezer tempera-
holder using the capsule loading unit. ture. Place 100 ml of carbon disulfide in the pressure bottle(s)
17.4.2 Injection of the Sample: to which other monomers have been added. Store in the freezer
and allow to come to temperature. Transfer the Bd to the
17.4.2.1 For Model 3920: Remove the capsule holder from
syringe and close the valve. Using an absorbent tissue, clean
the hot injector assembly and immediately align the capsule
the outside of the syringe, place in an insulator tube and weigh.
holder in the loading unit with capsule in the magazine. Press
Carefully inject the required amount of monomer into the
down on the capsule holder firmly until the capsule is seated in
pressure bottle below the liquid surface and mix. Withdraw the
the capsule holder. Be certain to remove any used capsule from
syringe, place in an insulator tube and re-weigh. The difference
the holder and instrument. Remove the capsule holder from the
is the amount of Bd injected. Prepare standards at about 0.01,
loading unit. Check for the conditions desired, and wait for the
0.04, 0.1, 0.3 and 0.7 grams per 100 ml of solvent. Any excess
green light to come on. The green light must be on before
monomer in the syringe should be vented to the outside air. The
inserting the sample. Gently and slowly insert the capsule
pressure bottle of Bd should also be vented to the outside air
holder containing the sample capsule, just short of puncturing
after standards have been tested. The samples are ready to be
the capsule. The capsule should be in the injection port to be
injected into the Gas Chromatograph.
heated. After 15 s, insert the capsule holder all the way into the
instrument to puncture the capsule. The forepart of the capsule
holder will be almost flush with the front of the instrument. 18. Precision and Bias
Immediately after injecting the sample, press the start button 18.1 This precision and bias section has been prepared in
on the integrator. Do not press the light on the chromatograph. accordance with Practice D4483. Refer to Practice D4483 for
After one minute, remove the capsule holder from the instru- terminology and other statistical calculation details.
ment. While the instrument is cooling, reinsert the capsule
18.2 The precision results in this precision and bias section
holder to keep it hot. When the door opens at the end of the
give an estimate of the precision of these test methods with the
testing cycle, press the button again to stop the integrator. Turn
materials (rubbers) used in the particular interlaboratory pro-
off the chart. When the instrument has cooled to the initial
gram as described below. The precision parameters should not
temperature, another sample can be injected. The integrator
be used for acceptance/rejection testing of any group of
prints out the elution time and the peak area, and the ppm of
materials without documentation that they are applicable to
each component of interest.
those particular materials and the specific testing protocols that
17.4.2.2 For Model Sigma 2: Set instrument for conditions
include these test methods.
desired, and wait for the oven ready light to come on. This light
and the start button must be lit before injecting the sample. 18.3 A Type 1 (interlaboratory) precision was evaluated.
Gently and slowly insert the capsule holder containing the Both repeatability and reproducibility are short term; a period

10
 D1417 − 16
TABLE 2 Type 1 Precision for Synthetic Rubber Latices—Various Tests
NOTE 1—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

of a few days separates replicate test results. Information on the by more than the tabulated r (for any given must be considered
number of laboratories and the materials used is given in Table to have come from different or nonidentical sample popula-
2. tions.
18.4 The results of the precision calculations for pooled 18.7 Repeatability and reproducibility expressed as a per-
repeatability and reproducibility are given in Table 2 for a cent of the mean level, (r) and (R), have equivalent application
broad series of test parameters. statements as above for r and R. For the (r) and (R) statements,
18.5 The precision of these test methods may be expressed the difference in the two single test results is expressed as a
in the format of the following statements which use an percent of the arithmetic mean of the two test results.
“appropriate value” of r, R, (r), or (R), to be used in decisions 18.8 Bias—In test method terminology, bias is the difference
about test results. The appropriate value is that value of r or R between an average test value and the reference (or true) test
associated with a mean level in Table 2 closest to the mean property value. Reference values do not exist for these test
level under consideration at any given time for any given test, methods, since the value (of the test property) is exclusively
for any given material in routine testing operations. defined by the test methods. Bias therefore cannot be deter-
18.6 Repeatability—The repeatability, r, of these test meth- mined.
ods has been established as the appropriate value tabulated in
Table 2. Two single test results, obtained in two different 19. Keywords
laboratories, under normal test method procedures, that differ 19.1 latex; rubber latices; synthetic

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