to600625°C for at least20min.Cool in a desiccator and weigh.
11.Calculation
11.1Calculate the percent ash as follows:
A5~B/C!3100(1) where:
A5ash,%,
35mm镜头
B5mass of ash,g,and
C5mass of sample,g.
12.Report
12.1Report the following information:
12.1.1Proper identification of the sample,and
12.1.2Results of two individual determinations and their average reported as percent ash to the nearest0.01%.
13.Precision and Bias3
13.1This precision and bias ction has been prepared in accordance with Practice D4483.Refer to Practice D4483for terminology and other statistical details.
13.2The 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-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.
13.3A Type1(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.
13.4Three different materials were ud in the interlabora-tory program.They were tested in ven laboratories on two different days.
13.5The results of the precision calculations for repeatabil-ity and reproducibility are given in Table1,in ascending order of material average or level,for each of the materials evalu-ated.
N OTE1—The percent ash values have been multiplied by100to avoid
leading zeros in Table1.The values of S
r ,r,S
R
,and R are influenced by
this multiplication factor,for example:S
r (percent ash times100)/
1005S
r
(actual or true percent ash basis).
13.6The 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 and R associated with a mean level in Table1clost to the mean level under consideration at any given time,for any given material in routine testing operations.
13.7Repeatability—The repeatability,r,of this test method has been established as the appropriate value tabulated in Table1.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.
13.8Reproducibility—The reproducibility,R,of this test method has been established as the appropriate value tabulated in Table1.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 OTE2—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.
石排湾公园13.9The relative repeatability(r)and reproducibility(R) have been omitted from Table1since 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.
13.10Bias—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.
ACCELERATORS AND ANTIDEGRADANTS
14.Scope
14.1This test method describes the determination of the ash content of accelerators and antidegradants.
15.Summary of Test Method
15.1The ash content is determined by heating a known quantity of material over a gas burner to remove organic material leaving a carbonaceous mass.Ashing is completed in a muffle furnace.The remaining ash,measured by mass difference,is expresd as a percent of the original material.
16.Significance and U
16.1The ash content of a sample is the amount of all noncarbon components that remain after combustion,indepen-dent of chemical form.In effect,the analysis measures residual
3Supporting data are available from ASTM Headquarters.Request RR:D11-1050.
TABLE1Precision Results—Ash,%,3100
Material Average
Within Laboratory A Between Laboratory A
S r r S R R Insoluble
Sulfur—A(Oil
Treated,90%)
0.390.3180.9010.507 1.43
General Purpo
Ground Sulfur
3.430.847 2.399 1.560
4.41
Insoluble
Sulfur—B(Oil
Treated,90%)
7.75 1.772 5.015 2.150 6.08
Pooled Values B 3.85 1.149 3.251 1.561 4.41
A S
r
5repeatability standard deviation.新郎发言
r5repeatability(2.833the square root of the repeatability variance).
S R5reproducibility standard deviation.
R5reproducibility(2.833the square root of the reproducibility variance).
B No values
omitted.
inorganic impurities that can remain with the product at low levels following the manufacturing process.
16.2The quantity of ash in accelerators or antidegradants can affect the performance of the additives in rubber if critical levels are exceeded.
17.Apparatus
17.1See Section6.
18.Sampling
18.1To ensure homogeneity,at least250g of the lot sample should be well blended prior to removing the test unit.
关于亲情的题记19.Procedure孤独的文章
19.1Ignite the15-cm3crucible in the muffle furnace at750 625°C for30min.
19.2Transfer the crucible to the desiccator,cool to room temperature and weigh to the nearest0.0001g.
19.3Weigh a5-g test unit to the nearest0.0001g into the ignited crucible.Place the crucible in the clay
triangle,and carefully heat the crucible and contents with the gas burner until all volatile material and pyrolysis products have been removed(gas mayflame)and the residue has been carbon-ized.
19.4Transfer the crucible to the muffle furnace at7506 25°C and ignite for2h.
19.5Carefully transfer the crucible containing the ash to the desiccator,cool to room temperature,and reweigh to the nearest0.0001g.
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19.6Repeat the procedure on a cond test unit.
20.Calculation
20.1Calculate the percent ash to the nearest0.01%as follows:
A5@~D2B!/~C2B!#3100(2) where:年度考核领导考核评语
A5ash,%,
B5mass of crucible,g,
C5mass of crucible plus test unit,g,and
D5mass of crucible plus the ash,g.
21.Report
21.1Report the following information:
21.1.1Proper identification of the sample,and
21.1.2Results obtained from two individual determinations and their average,reported to the nearest0.01%.
22.Precision and Bias3
22.1This precision and bias ction has been prepared in accordance with Practice D4483.Refer to Practice D4483for terminology and other statistical details.
22.2The 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-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.
22.3A 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.
22.4Six different materials were ud in the interlaboratory program.The were tested in ven laboratories on two different days.
22.5The 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.
22.6The 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 Table2clost to the mean level under consideration at any given time,for any given material in routine testing operations.
22.7Repeatability—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.
22.8Reproducibility—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.
22.9The 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.
22.10Bias—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. 23.Keywords
23.1ash;rubber chemicals
TABLE2Ash Content,PPD Antidegradants and Accelerators,% Material
Aver-
age
Within Laboratory A Between Laboratory A
S r r S R R
M1-6PPD0.020.0120.0330.0130.036
M2-IPPD0.010.0040.0130.0090.026
M3-BMPPD0.010.0070.0200.0120.034
M4-DTPD0.020.0050.0150.0080.025
M5-DCBS0.030.0020.0060.0070.020
M6-TBBS0.050.0050.0160.0090.027 Pooled values B0.020.0070.0200.0100.028
A S
r
5repeatability standard deviation.
r5repeatability(2.833the square root of the repeatability variance).
S R5reproducibility standard deviation.
R5reproducibility(2.833the square root of the reproducibility variance).
B No values
搞怪短信
omitted.
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