Remove the specimen,cover,and cool in a desiccator for 1h.
Weigh the cooled specimen to the nearest 0.1mg.
12.Calculation
12.1The volatile material is given by the following equa-
tion:
V 5~S o !2~S h !/S o 3100(1)
where:V 5volatiles,%,S o 5original specimen mass,and
S h 5heated specimen mass.
13.Report
13.1Report results obtained from two individual determi-
nations and their average to the nearest 0.01%.
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14.Precision and Bias 3
14.1This precision and bias ction has been prepared in
accordance with Practice D 4483.Refer to Practice D 4483for
terminology and other statistical details.
14.2The precision results in this precision and bias ction
give an estimate of the precision of this test method with the
materials (rubbers)ud in the particular interlaboratory pro-gre高分作文
grams as described below.The precision parameters should not
be ud for acceptance/rejection testing of any group of
materials without documentation that they are applicable to
tho particular materials and the specific testing protocols that
include this test method.
14.3A Type 1(interlaboratory)precision was evaluated in
1986.Both repeatability and reproducibility are short term.A
period of a few days parates replicate test results.A test result
is the mean value,as specified by this test method,obtained on
two determinations or measurements of the property or param-
eter in question.
14.4Three different materials were ud in the interlabora-
tory program.The were tested in ven laboratories on two
different days.
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14.5The results of the precision calculations for repeatabil-
ity and reproducibility are given in Table 1,in ascending order
of material average or level,for each of the materials evalu-
ated.
14.6The precision of this test method may be expresd in the format of the following statements which u an “appro-priate value”of r,R ,(r )or (R ),that is,that value to be ud in decisions about test results (obtained with the test method).The appropriate value is that value of r or R associated with a mean level in Table 1clost to the mean level under consideration at any given time,for any given material in routine testing operations.14.7Repeatability —The repeatability,r ,of this test method has been established as the appropriate value tabulated in Table 1.Two single test results,ob
tained under normal test method procedures,that differ by more than this tabulated r (for any given level)must be considered as derived from different sample populations.14.8Reproducibility —The reproducibility,R ,of this test method has been established as the appropriate value tabulated in Table 1.Two single test results obtained in two different laboratories,under normal test method procedures,that differ by more than the tabulated R (for any given level)must be considered to have come from different or nonidentical sample populations.N OTE 1—The values of r and R are relatively large,whereas the average or mean test level is small (clo to zero).This is typical for this type of precision measurement process.This should be kept in mind whenever u is made of r and R .14.9The relative repeatability (r )and reproducibility (R )have been omitted from Table 1since the level of values tested was extremely low and approached the limits of nsitivity of the test method.Under the circumstances the relative values become trivial.14.10Bias —In test method terminology,bias is the differ-ence between an average test value and the reference (or true)test property value.Reference values have not been evaluated for this test method.Bias,therefore,cannot be determined.p -PHENYLENEDIAMINE ANTIDEGRADANT 15.Scope 15.1This test method describes the determination of vola-tile materials in p -phenylenediamine antidegradants and is bad on the mass loss upon heating at 70°C.15.2The measured loss on heating reprents volatile or-ganics plus moisture.16.Summary of Test Method 16.1The p -phenylenediamine test unit is weigh
ed before and after heating for 3h at 70°C.The measured difference in mass is the volatile material.17.Significance and U 17.1The quantity of volatile material in p -phenylenediamines can affect performance of the anti-degradants in rubber if they exceed critical levels.17.2Since the loss on heating is an empirical and nonspe-cific method,it is esntial that the prescribed analysis condi-tions (sample container,oven temperature,oven air flow,cooling conditions,etc.)be controlled so that results are meaningful.17.3Prolonged heating or overheating of the sample or the
3Supporting data are available from ASTM Headquarters.Request RR:D11-
1047.TABLE 1Type 1Precision Results—Volatile Materials,Percent
Material Aver-age Within Laboratory A Between Laboratory A
2009考研英语真题
S r r S R R
General Purpo Ground Sulfur
0.070.0180.0530.0450.127
Oil Treated,90%Insolule Sulfur—A
0.260.0250.0730.1300.368
Oil Treated,90%Insoluble Sulfur—B
depositary0.320.0420.1190.1510.427
Pooled Values B 0.220.0300.0870.1190.338
A S r 5repeatability standard deviation.
r 5repeatability 52.833the square root of the repeatability variance.
S R 5reproducibility standard deviation.
R 5reproducibility 52.833the square root of the reproducibility variance.
B No values
omitted.
test unit can result in high heat loss values due to oxidative generation of volatile degradation products.
18.Apparatus
18.1See Section6.
19.Sampling
19.1To ensure homogeneity,at least250g of the“lot”sample should be well blended prior to removing the test unit.
20.Procedure
20.1Dry a clean weighing bottle and stopper(stopper removed)for30min in the specified oven t at70°C.Place the bottle and stopper in the desiccator and allow them to cool to room temperature.Weigh the bottle with a stopper to the nearest0.1mg.
成人高考准考证怎么打印20.2Weigh a nominal20-g test unit into the weighing bottle to the nearest0.1mg.
20.3Place the weighing bottle containing the test unit and the stopper(with the stopper removed)in the specified oven, which has equilibrated at70°C,for3h.
20.4After the heating period,replace the stopper and transfer the bottle to the desiccator for a period of time sufficient for the asmbly to equilibrate at room temperature. Reweigh the bottle to the nearest0.1mg.
20.5Repeat the procedure on a cond test unit.
21.Calculation
21.1Calculate the percent heating loss to the nearest0.1% as follows:
H5@~B2C!/~B2A!#3100(2) where:koei
H5heating loss,%,
A5mass of weighing bottle and stopper,g,
B5mass of weighing bottle,stopper,and test unit before heating,g,and
C5mass of weighing bottle,stopper,and test unit after heating,g.
22.Report
22.1Report the following information:
22.1.1Proper identification of the sample,andronan
22.1.2Results obtained from two individual determinations and their average,reported to the nearest0.01%.
23.Precision and Bias3
23.1This precision and bias ction has been prepared in accordance with Practice D4483.Refer to Practice D4483for terminology and other statistical details.
23.2A Type1(interlaboratory)precision was evaluated in 1987.Both repeatability and reproducibility are short term.A period of a few days parates replicate test results.A test result is the mean value,as specified by this test method,obtained on two determinations or measurements of the property or param-eter in question.
23.3Four different materials were ud in the interlabora-tory program.The were tested in six laboratories on two different days.
23.4The results of the precision calculations for repeatabil-ity and reproducibility are given in Table2,in ascending order of material average or level,for each of the materials evalu-ated.
23.5The precision of this test method may be expresd in the format of the following statements which u an“appro-priate value”of r,R,(r),or(R),that is,that value to be ud in decisions about test results(obtained with the test method). The appropriate value is that value of r or R associated with a mean level in Table2clost to the mean level under consideration at any given time,for any given material in routine testing operations.
23.6Repeatability—The repeatability,r,of this test method has been established as the appropriate value tabulated in Table2.Two single test results,obtained under normal test method procedures,that differ by more than this tabulated r (for any given level)must be considered as derived from different or nonidentical sample populations.
23.7Reproducibility—The reproducibility,R,of this test method has been established as the appropriate value tabulated in Table2.Two single test results obtained in two different laboratories,under normal test method procedures,that differ by more than the tabulated R(for any given level)must be considered to have come from different or nonidentical sample populations.
23.8The relative repeatability(r)and reproducibility(R) have been omitted from Table2since the level of values tested was extremely low and approached the limits of nsitivity of the test method.Under the circumstances the relative values become trivial.
23.9Bias—In test method terminology,bias is the differ-ence between an average test value and the reference(or true) test property value.Reference values have not been evaluated for this test method.Bias,therefore,cannot be determined.
24.Keywords
24.1antidegradants;rubber chemicals;sulfur;volatile con-tent
TABLE2Volatile Materials of p-Phenylenediamine,Percent
Material
Aver-
age
Within Laboratory A Between Laboratory A
S r r S R R
M1-6PPD0.060.0220.0620.0290.083
M2-IPPD0.080.0040.0110.0260.075
M3-BMPPD0.190.0340.0980.0730.026
M4-DTPD0.040.0020.0050.0190.055 Pooled Values B0.090.0210.0610.0450.129
A S
r
5repeatability standard deviation.考研政治考试时间
r5repeatability52.833the square root of the repeatability variance.kisi
S R5reproducibility standard deviation.
R5reproducibility52.833the square root of the reproducibility variance.
B No values
omitted.
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