本标准规定了采用ASTM标准参比炭黑(SRBs)连续监控炭黑试验方法精密度的方法和用统计控制图来确定本实验室的SRBｓ试验结果与其确认值是否有显著性差异的方法，并指出可能影响试验精密度的原因。本标准适用于实验室内确认其炭黑试验方法的精密度和偏差是否达到标准要求，也适用于找出并消除影响试验精密度的原因，经校正后使试验精密度达到标准要求。 GB/T 15338-1994 炭黑试验方法精密度和偏差的确认 GB/T15338-1994 标准下载解压密码：www.bzxz.net

National Standard of the People's Republic of China
Confirmation of test method precision and bias of carbon blackStandard guide for cerbon black-Valldatlon of test method precision and bias1Subject content and scope of application
GB/T15338-94
This standard specifies the method for continuously monitoring the precision of carbon black test methods using ASTM standard reference carbon black (SRB) and the method for using statistical control charts to determine whether the SRBs test results of this laboratory are significantly different from their confirmed values, and points out the reasons that may affect the test precision.
This standard is recommended for confirming whether the precision and deviation of the carbon black test method meet the standard requirements in dry experiments, and it is also suitable for finding and eliminating the reasons that affect the test precision. After calibration, the test precision reaches the standard requirements. 2 Reference standards
Carbon black iodine absorption value test method for rubber
GB/T 3780.1
GB/ T3780.2 Determination of butyl phthalate absorption value of carbon black (A method) GB/T3780.4 Carbon black (compressed sample) Dibutyl phthalate absorption value determination method and sample preparation carbon black specific surface area determination CTAB method GB/T 3780.5
GB/T3780.6 Carbon black coloring intensity for rubber Test method GB/T10722 Determination of specific surface area of ​​carbon black Nitrogen adsorption method GB/T1.0723 Standard method for improving the reproducibility of carbon black with ASTM standard 3 steps
3.1 According to the method of Appendix A, for each test method, a control chart is prepared for each SRBs. 3.2 The target values ​​in Table 1 are standard values ​​of SRBs. These values ​​plus or minus 3 times the standard deviation of the single test repeatability specified in the test method serve as the upper and lower limits of the control chart.
3.3 Use the selected test method (see Chapter 2) to continuously test the six SRBs regularly or irregularly, and fill in the test values ​​in the control chart. If the test values ​​are all within the control limits, it can be confirmed that the precision and deviation of this test in this laboratory are valid: If the test value of one of the SRBs exceeds the repeatability control limit, the six SRBs should be retested immediately. The State Administration of Technical Supervision approved 1994-12-22 to implement 1995-09-01
Iodine absorption value,
DBP absorption value,
10-*m/kg
(cm/100g)
CDBP acquisition value,
10-5m/kg
(cm2/100g)||tt t||CTAB surface area:
10°m/kg
(m°/g)
Test method
GB/T 3780.1
GB/T 3780.2
GB/T 3780.4
GB/T 3780.5
GB/T15 338—94
Table 1 control diagram boundary
target value
control drawing rejuvenation 3S boundary
ammonia area,
10°m/kg
color intensity
test method
GB/T 10722
GB/T 3780.6||t t||GB/T1533B—94
continued Table 1
Target value
Control chart reconciliation 3 S boundary
3. 4 If the retested SRBs test results still fall outside the repetitive control limit, start looking for the reasons that may affect the precision of the test (see possible reasons listed in Chapter 4). 3.5 If after finding the possible causes and taking appropriate corrective measures, the test results still cannot fall within the control limits, the regression equation, i.e. the correction equation, shall be calculated according to the method specified in GB/T 10723. 3.6 Continuously monitor all SRBs and use the 4 most recent data of each SRB to establish the correction equation. Otherwise, the calibration equation will not be comparable with calibrations already performed in other laboratories or with other instruments. 3.7 Continue testing each SRB and calibrate all test results using the established calibration equations and plot the calibration values ​​on the control chart. When one test result exceeds the control limit, a retest is performed immediately. If the average of the two test values ​​still falls outside the control limit, the statistical correction equation is recalculated and determined using the four latest test data for each SRBs. 3.B If the data corrected with the new calibration equation still fall outside the repeatability control limits, the test method should be discontinued until the corrective measures taken can make the SRB: carbon black test results fall within 3 times the repeatability standard deviation control limits. Note: This chapter specifies only the minimum measures required for continuous monitoring of the accuracy of the test face method. 3.9 Use SRBs A-4, B-4; C-4, D-4, E-4 and F-4. See Appendix B for examples of correction equations for determining DBP absorption values. 3.10 Examples of control diagrams for 6 types of SRBs are given in Appendix A. 4 Possible reasons affecting test precision
4.1 The following are possible reasons why the precision of the test method exceeds the range of the statistical control chart. 4.1.1 GB/T 3780.1 Iodine absorption value test method: 4.1.1.1 The concentrations of iodine and sodium thiosulfate solutions are inaccurate; 4.1.1.2 The glass measuring instrument is not calibrated;
4.1.1.3 The purity of water is not enough:
4.1.1.4 The size of the pipette used is not appropriate 4.1.1.5 Wash or rinse the glassware with unclean water. GB/T 15338--94
4.1.2GB/T3780.2DBP absorption value test method:4.1.2.1The cooling time between samples is inconsistent;4. 1. 2. 2
Improper installation of torsion spring and retaining ring:
4. 1.2. 3
4. 1.2. 5
4. 1. 2. 7
Improper installation of torque limit switch:
The gap between rotor and mixing chamber is too large;
The surface finish of filling chamber is not smooth enough,
The buffer oil level is incorrect;
DBP titration flow rate or flow is inappropriate:
There are bubbles in DBP burette;
4.1.2.9Improper cleaning and lubrication between rotor and mixing chamber. 4.1.3GB/T3780.4CDBP absorption value test method: 4.1.3.1
4.1.3.3
Opposite to 4.1.2:
The compression system pressure is not calibrated;
The number of compressions is incorrect.
4.1.4GB/T3780.CTAB surface area test method 4. 1- 4. 1
The ITRB used as the standard is incorrect;
4.1.4.2The pressure of the filter branch is inaccurate:; 4.T.4.3The pore size of the filter membrane is incorrect;
The calibration curve is not checked daily;
4.1.4.5The illumination of the automatic titrator is not enough. 4.1.5 GB/T3780.6 Tinting strength test method: 4.1.5.1 The ITRB carbon black used is incorrect or contaminated; 4. 1. 5. 2
The number of grinding times is incorrect:
The glass plate of the grinder is excessively scratched or uneven; 4. 1. 5. 3
4.1.5.4 The reflectometer is not calibrated.
4. 1-6 GB/T 10722
2 Test method for nitrogen adsorption surface area;
4.1.6.1 Instrument is full of air:
4.1.6.2 The type 0 bacteria used are unqualified.
method; For all test methods, if one SRB is suspected to be contaminated or to have abnormal aging deterioration, other SRB samples should be used. 5 Determination of Precision and Bias
5.1 For a test method, the bias of a SRB for multiple tests can be determined by the difference between the average value X of the 25 most recent test results (including corrected, uncorrected, or both) and the ASTM confirmed value (X-XASTM). 5.2 For a test method, the precision of a SRB test may be determined by calculating the standard deviation S of the 25 points in 5.1. (X - X)?+. +(X, -x)*
6 Test report
6.7 The test report shall include the following contents:
Test method standard number:
b. Deviation (X-XAsTM) value determined according to 5.1: C. Deviation (X-XAsTM) value determined according to 5.2 determined standard deviation value S.
Experimental determination:
Operator:
Date:
Time,
Sample apparent value
Average value ()
Instrument:
71.170. 671.470. 77624
GB/T 15338—94
Appendix A
DBP absorption value control chart example
(supplement)
Quantity control
Test method GB/T3780.2
Target value:
Drawing number:
Specification specification: 70. 8±0.95
Measurement unit,
SRB A-4 Control Chart
Season adjustment,
Original data
Calibration data
Laboratory:
Operator:
Time,
Scientific product measurement position
Instrument:
1 100. 499. 211.999. 559.9
Average value (
GB/T 15338—94
Test method; GB/T 3780.2
Target value:
Drawing number:
Specification range: 100±1.37
Measurement unit,
Original data
Calibration data
17181920212223 24
Figure A2SRBB-4 Control Chart
Experimental host:
Operator:
Order period:
Time:
Group product value
Average value
Range R
GB/T 15338—94
Test piece method GB/T3780.2
Target value:
Specification range: 13F.8±1.45
Maximum unit:
Initial data
Calibration data
22232425
Figure A3SRBC-4 control chart
.Upper limit
Laboratory:
Operator;
Time:
Sample maximum value
Average value (yuan)
Range R
GB/T 15338—94
Variable control
Test method: GB/T378m.2
Daily standard value:
SRB,D 4
Drawing number:
Specification range: 64. 8=1. 31
Unit of measurement
Original data
Correction data
17181920
Figure A4SRBT-4 control chart
. Upper crack
Test room:
Workbook,
Time,
Scientific product measurement value
an.7go.991.aaa.3n.4
Average value()
GB/T15338—94
Test method B/19780.2
Monthly standard value:
SRB,E- 4
Drawing number,
Specification range: 90.1±2.24
Zero adjustment,
Measurement unit:
Initial data
Positive data
Figure A5SRBF-4 control chart
Laboratory
Operator
Date,
Sample measurement value
GB/T15338—94
Test method: GB/T_9780.2
Use standard value,
151. 023. 4:16. 629.1: 30. :2
Average value (x)
Chart number,
Specification range: 190.0-1.91
Measurement unit:
Zero adjustment,
Initial data
Correction data
18192021282324
151617
SRB F-4 control chart
. Upper limit
B1 correction equation model
-standard value:
Where: Y—
A——slope;
X——measured value;
B-intercept.
Formula (B1) can be transformed into:
B2 Calculation correction equation
Find A and B (using the least square method)
Measurement!
GB/T 15338—94
Appendix B
DBP absorption value correction equation calculation example
(reference)
Y-AX +B
CV(correction value)=A(measured value)+B
Measured value and standard value of DBP absorption value and calculation of A and B B-4
ZX=2 344. 8,ZY -2 34G. 0,EXY -=245 197. 7
2x3-245061.4,2P2=245 353.3.n=24B(cut)
A(slope)
nEX2-(EX)
nEXY-EXEY
NEX-(EX)
-0.066 6—0.1
Note: ASTM1) 4821-92 reversed X and Y in the calculation, and the result was also wrong when substituting A (material rate) and B (intercept). This standard has made corrections. B2.2 Calculate the correction equation
Substitute the A and B values ​​obtained in B2.1 into equations (B1) and (B2) to obtain: Y=1.001x-0.1
CV-1.001(measured value)-0.1
B2.3 Example
If the test value of SRBB4 is 99.9, then its correction value is: CV - 1.001X 99.9-0.1 - 99.9(B1)
Additional instructions
GB/T1538-94
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Black Industry Research and Design Institute of the Ministry of Chemical Industry. This standard was drafted by the Black Industry Research and Design Institute of the Ministry of Chemical Industry. The main drafters of this standard are Chen Junqiu and Hu Kaishu. This standard is equivalent to the American Society for Testing and Materials standard ASTMD82-92 black test method density and deviation are indeed the same as the American methodUpper limit
Laboratory:
Operator;
Time:
Sample sub-maximum value
Average value (yuan)
Range R
GB/T 15338—94
Variable control
Test method: GB/T378m.2
Daily standard value:
SRB,D 4
Drawing number:
Specification range: 64. 8=1. 31
Unit of measurement
Original data
Correction data
17181920
Figure A4SRBT-4 control chart
. Upper crack
Test room:
Workbook,
Time,
Scientific product measurement value
an.7go.991.aaa.3n.4
Average value()
GB/T15338—94
Test method B/19780.2
Monthly standard value:
SRB,E- 4
Drawing number,
Specification range: 90.1±2.24
Zero adjustment,
Measurement unit:
Initial data
Positive data
Figure A5SRBF-4 control chart
Laboratory
Operator
Date,
Sample measurement value
GB/T15338—94
Test method: GB/T_9780.2
Use standard value,
151. 023. 4:16. 629.1: 30. :2
Average value (x)
Chart number,
Specification range: 190.0-1.91
Measurement unit:
Zero adjustment,
Initial data
Correction data
18192021282324
151617
SRB F-4 control chart
. Upper limit
B1 correction equation model
-standard value:
Where: Y—
A——slope;
X——measured value;
B-intercept.
Formula (B1) can be transformed into:
B2 Calculation correction equation
Find A and B (using the least square method)
Measurement!
GB/T 15338—94
Appendix Bwww.bzxz.net
DBP absorption value correction equation calculation example
(reference)
Y-AX +B
CV(correction value)=A(measured value)+B
Measured value and standard value of DBP absorption value and calculation of A and B B-4
ZX=2 344. 8,ZY -2 34G. 0,EXY -=245 197. 7
2x3-245061.4,2P2=245 353.3.n=24B(cut)
A(slope)
nEX2-(EX)
nEXY-EXEY
NEX-(EX)
-0.066 6—0.1
Note: ASTM1) 4821—92 reversed X and Y in the calculation, and the result was also wrong when substituting A (material rate) and B (intercept). This standard has made corrections. B2.2 Calculate the correction equation
Substitute the A and B values ​​obtained in B2.1 into equations (B1) and (B2) to obtain: Y=1.001x-0.1
CV-1.001(measured value)-0.1
B2.3 Example
If the test value of SRBB4 is 99.9, then its correction value is: CV - 1.001X 99.9-0.1 - 99.9(B1)
Additional instructions
GB/T1538-94
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Black Industry Research and Design Institute of the Ministry of Chemical Industry. This standard was drafted by the Black Industry Research and Design Institute of the Ministry of Chemical Industry. The main drafters of this standard are Chen Junqiu and Hu Kaishu. This standard is equivalent to the American Society for Testing and Materials standard ASTMD82-92 black test method density and deviation are indeed the same as the American methodUpper limit
Laboratory:
Operator;
Time:
Sample sub-maximum value
Average value (yuan)
Range R
GB/T 15338—94
Variable control
Test method: GB/T378m.2
Daily standard value:
SRB,D 4
Drawing number:
Specification range: 64. 8=1. 31
Unit of measurement
Original data
Correction data
17181920
Figure A4SRBT-4 control chart
. Upper crack
Test room:
Workbook,
Time,
Scientific product measurement value
an.7go.991.aaa.3n.4
Average value()
GB/T15338—94
Test method B/19780.2
Monthly standard value:
SRB,E- 4
Drawing number,
Specification range: 90.1±2.24
Zero adjustment,
Measurement unit:
Initial data
Positive data
Figure A5SRBF-4 control chart
Laboratory
Operator
Date,
Sample measurement value
GB/T15338—94
Test method: GB/T_9780.2
Use standard value,
151. 023. 4:16. 629.1: 30. :2
Average value (x)
Chart number,
Specification range: 190.0-1.91
Measurement unit:
Zero adjustment,
Initial data
Correction data
18192021282324
151617
SRB F-4 control chart
. Upper limit
B1 correction equation model
-standard value:
Where: Y—
A——slope;
X——measured value;
B-intercept.
Formula (B1) can be transformed into:
B2 Calculation correction equation
Find A and B (using the least square method)
Measurement!
GB/T 15338—94
Appendix B
DBP absorption value correction equation calculation example
(reference)
Y-AX +B
CV(correction value)=A(measured value)+B
Measured value and standard value of DBP absorption value and calculation of A and B B-4
ZX=2 344. 8,ZY -2 34G. 0,EXY -=245 197. 7
2x3-245061.4,2P2=245 353.3.n=24B(cut)
A(slope)
nEX2-(EX)
nEXY-EXEY
NEX-(EX)
-0.066 6—0.1
Note: ASTM1) 4821—92 reversed X and Y in the calculation, and the result was also wrong when substituting A (material rate) and B (intercept). This standard has made corrections. B2.2 Calculate the correction equation
Substitute the A and B values ​​obtained in B2.1 into equations (B1) and (B2) to obtain: Y=1.001x-0.1
CV-1.001(measured value)-0.1
B2.3 Example
If the test value of SRBB4 is 99.9, then its correction value is: CV - 1.001X 99.9-0.1 - 99.9(B1)
Additional instructions
GB/T1538-94
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Black Industry Research and Design Institute of the Ministry of Chemical Industry. This standard was drafted by the Black Industry Research and Design Institute of the Ministry of Chemical Industry. The main drafters of this standard are Chen Junqiu and Hu Kaishu. This standard is equivalent to the American Society for Testing and Materials standard ASTMD82-92 black test method density and deviation are indeed the same as the American method
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