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GB 17378.2-2007: The specification for marine monitoring -- Part 2: Data processing and quality control of analysis
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Basic data | Standard ID | GB 17378.2-2007 (GB17378.2-2007) | | Description (Translated English) | The specification for marine monitoring -- Part 2: Data processing and quality control of analysis | | Sector / Industry | National Standard | | Classification of Chinese Standard | A45 | | Classification of International Standard | 07.060 | | Word Count Estimation | 38,374 | | Date of Issue | 2007-10-18 | | Date of Implementation | 2008-05-01 | | Older Standard (superseded by this standard) | GB 17378.2-1998 | | Quoted Standard | GB/T 8170; GB 17378.5-2007; GB 17378.6-2007 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 12 of 2007 (total 112) | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This Chinese standard relates to marine monitoring data processing provides common terms and symbols, outliers statistical tests, two significant differences in the mean test, validation of analytical methods, sample preparation and application of internal control, analytical quality control drawing and so on. For analysis of marine environmental monitoring in seawater, sediment analysis, biological analysis, coastal pollution and biological monitoring of ecological survey data processing and analysis of laboratory internal quality control. | GB 17378.2-2007: The specification for marine monitoring -- Part 2: Data processing and quality control of analysis
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The specification for marine monitoring.Part 2. Data processing and quality control of analysis
ICS 07.060
A45
National Standards of People's Republic of China
Replacing GB 17378.2-1998
Marine monitoring
Part 2. Data processing and quality control analysis
Posted 2007-10-18
2008-05-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Table of Contents
Introduction Ⅲ
1 Scope 1
2 Normative references 1
3 Terms and definitions
3 4 General provisions
5 Data Processing 4
5.1 significant digits and rounding off 4
5.2 statistical outlier test 7
Significant differences between the two sets of data test 5.3 11
Internal analytical quality control laboratory 6 17
17 6.1 Validation of Analytical Procedures
6.2 Sample preparation and application of internal control 23
6.3 Quality Control Chart Analysis 23
Appendix A (informative) seawater analysis blank upper detection limit, detection limit estimated 31
A. 1 calibration curve estimation method 31
A. 2 blank assay standard deviation 32
Figure 1 Calibration curve 21
The basic composition of 24 2 Control Charts
Figure 3 Mean control (Ken X) showing the basic composition of 24
Figure 4 Mean Control (Ken X) Figure Example 25
5 mean - range control (Ken XR) Figure 27 basic components
Figure 6 mean - range control (Qin X-R) Figure Example 27
7 29 Recovery control
Table 1 seawater parallel twin-like relative deviation Table 4
Table 2 Recovery allowable value Table 4
First Table 3 minutes without pipettes accurate representation capacity 6
Table 4 equal amounts into a flask formula accurate representation capacity 6
Table 5 Dixon test statistic (Q) formula 8
Table 6 Dixon test threshold (Qα) Table 8
Table 7 Grubbs test threshold (Tα) value of 10
Table 8 Cochran maximum variance test threshold (Cα) Table 11
Table 9 for each field of application of the formula 13
Table 10 Determination of the new law and the results of the original law 13
Table 11 groups Found 14
Determination method results in Table 12 B 15
Table 13 recoveries were 16 results
Determination of mercury concentration values in Table 14 17
Table 15 F value (significance level of P = 0.05) 18
Table 16 F value (significance level P = 0.01) 18
Table 17 calibration curves recorded statistics 21
Table 18 precision, accuracy verification records 22
25 Table 19 measurement results
Table 20 control chart coefficient table (like parallel samples each measurement) 26
Table 21 Table 29 active phosphate measurement data
Foreword
All technical content in this section is mandatory.
GB 17378 "marine monitoring" is divided into seven parts.
--- Part 1. General;
--- Part 2. Data processing and analysis of quality control;
--- Part 3. Sample collection, storage and transport;
--- Part 4. Seawater analysis;
--- Part 5. Sediment analysis;
--- Part 6. Analysis of the organism;
--- Part 7. Ecological survey of offshore pollution and biological monitoring.
This section GB 17378 Part 2, instead of GB 17378.2-1998 "specification for marine monitoring Part 2. Data processing and
Analytical quality control. "
This section compared with GB 17378.2-1998 main changes are as follows.
--- Amend the relevant provisions of the general regulations (1998 edition, Chapter 4; Chapter 4 of this edition);
--- Revised and improved the standard blank definition (1998 Version 3.6; 3.4 edition);
--- Again given the sensitivity of the method definition (1998 Version 3.11; edition 3.9);
--- Revised the detection limit, the lower limit of the measurement concept more clearly the meaning of these two concepts of probability (the 1998 edition 3.12,1.13; this
Version 3.10, 3.11);
--- Precision in the definition, and supplement its usual metric (1998 Version 3.17; 3.13 edition);
--- Gives a more precise definition of the system error and random error (the 1998 edition 3.29,3.30; this edition 3.25,3.26);
--- Increase the "value" is defined, for the inaccurate definition of significant figures were revised (1998 edition 5.1.1; 5.1.1 edition);
--- Unified regulations of the exponential form containing a plurality of targeting only play the role of "0" is a valid representation of a number (see 5.1.1);
--- Approximate calculation rules to an active digital computing rules (the 1998 edition 5.1.3; 5.1.3 edition);
--- Clear outliers and suspicious relationship between the data (1998 edition 5.2; 5.2 edition);
5.3.1.1);
--- Revised method for estimating the detection limit, standard deviation increase in the blank determination (see A.2).
Appendix A of this section is an informative annex.
This part by the State Oceanic Administration.
This part of the National Standards Technical Commission for Oceanography (SAC/TC283) centralized.
This section drafted by. National Marine Environmental Monitoring Center.
The main drafters of this section. Yu Tao, Zhang Chunming, mountain - foot plain, Xuheng Zhen, Han Dragon, Guan Tao Ming Ong Jian Guo, Chen Banglong, Li Nailan,
Xu Weilong.
This part of the standard replaces the previous editions are.
--- GB 17378.2-1998.
Marine monitoring
Part 2. Data processing and quality control analysis
1 Scope
GB 17378 of the provisions of this part of the ocean monitoring data processing commonly used terms and symbols, statistical tests outliers, the mean difference between two
The significance test, validation of analytical methods, sample preparation and application of internal control, analytical quality control drawing and the like.
This section applies to the marine environment monitoring analysis of seawater, sediment analysis, biological analysis, ecological survey offshore pollution and biological monitoring
Data Processing and Analysis laboratory internal quality control. Oceanic and Atmospheric pollutants into the sea fluxes survey, dredging and marine dumping investigation was also
Reference may be used.
2 Normative references
The following documents contain provisions which, through reference in this Part of GB 17378, constitute provisions of this part. For dated reference documents
Member, all subsequent amendments (not including errata content) or revisions do not apply to this section, however, encouraged to reach under this section
Parties to research agreement to use the latest versions of these documents. For undated reference documents, the latest versions apply to this
section.
GB 8170 numerical rounding rules
GB 17378.5-2007 marine monitoring Part 5. Sediment analysis
GB 17378.6-2007 marine monitoring Part 6. Analysis of the organism
3 Terms and Definitions
The following terms and definitions apply to this part of GB 17378.
3.1
Initial sample collection site.
3.2
Pretreated need to carry out sample measurement.
3.3
Independent samples taken from the same two or more samples.
3.4
Zero concentration corresponding to the standard series of analytical signal response.
3.5
In full agreement with the conditions of sample analysis, measurement results of blank samples.
3.6
The magnitude of the test signal value of the sample items (X) and analytical instruments given a correlation curve (Y) between. Calibration curves are divided into standard song
Line and curve.
3.7
Determination of the sample analysis process steps are identical to the standard series measured under the conditions of the calibration curve obtained.
3.8
Calibration curves measured under standard measuring step series of somewhat more than sample analysis process is simplified conditions.
3.9
Sensitivity of a measuring method, equal in magnitude response indicates that the amount of the signal and the signal generated test substance concentration or mass
Ratio. It reflects the degree of change in the concentration of the test substance units or units of quality changes resulting response signal indicative amount.
3.10
By one measurement can be 95% confidence probability qualitative judgment there is a minimum concentration or amount of material required for the test.
3.11
Confidence probability is 95%, the lowest concentration or the minimum amount can be measured quantitatively measured object.
3.12
The measurement results below the detection limit of XN.
3.13
Under specified conditions, the degree of mutual agreement between independent test results. Common standard deviation to measure.
Note. Precision depends only on the random error, and has nothing to do with the value of true value is measured or other agreement.
3.14
Sample difference between maximum and minimum values of the measurement results.
3.15
Each single difference between the measured value and the average value.
3.16
Single difference between the average value measured and then the average ratio.
3.17
Squared divided by the sample size and sample weight difference between the sample mean and the square root of minus 1, see equation (1).
S = 1 state -1Σ
2 (1)
Where.
S --- standard deviation;
X --- the average;
--- Like repetition number of measurements;
When the shape ≥20 time. S = 1 state Σ
2.
3.18
Sample standard deviation and sample mean ratio.
3.19
Under repeatability conditions, the degree of agreement between independent test results of.
3.20
In the same laboratory by the same operator using the same equipment, the same testing methods, and in a short time from the same measured object
Independent test results obtained conditions.
3.21
Under reproducibility conditions, the degree of consistency between the results of the test.
3.22
In different laboratories by different operators using different equipment, the same testing methods, to obtain the same from the test object to be measured
The results of the condition.
[GB/T 20001.4-2001, the definition 3.14]
3.23
The test results are consistent with the degree of the true value of measuring true or conventions.
3.24
The test results and the true value is measured (or conventional true value) of the difference. Including system test error and random error.
3.25
Measurement errors caused by determining one or more causes.
Note. Whatever the reason cause system errors are known or unknown, in theory, should be corrected using appropriate methods.
3.26
Uncertainty caused by the reason, obey the laws of statistics, with compensation of measurement errors.
NOTE. should reduce the effect of random errors on the measurement results through multiple measurements averaging method.
4 General Provisions
4.1 original site work record on the specified form with a hard pencil, writing correct, should not apply. Need to correct wrong note when, in the wrong
Uniform numbers on the horizontal line, write the correct figure up above it.
4.2 5.1 according to the method given in the recording and rounding the effective number of digits.
4.3 indicates that the test result and the dimensionless number of significant digits, indicate according to the analysis method specified. Without this provision, the a
Is a general principle of data only allowed at the end of a number is estimated (suspicious) value each other numbers are valid (credible), and so the decision
And an integer number of decimal places. Mandatory due to changes in dimension without decimals to take place, the details of the calculation method, see Chapter 5.
4.4 XN below the detection limit of the test results should be reported "not detected", but in the regional monitoring detection rate accounted for more than half the sample frequency (including
1/2) or less than 1/2, 1/2 and 1/4 portions were taken XN amount of undetected participate statistical operation.
4.5 Data not performed the competent department under the quality control program generated data considered suspect. Suspicious data can not be used for offshore
Environmental quality and marine environmental impact assessment.
4.6 parallel sample test is one way of analytical quality control. Principles laid down, not with the kind of simultaneous determination of internal projects, all bis test
Parallel analysis of samples. Dissolved oxygen, water, oil, etc. to be measured parallel to double the original sample (these do not need to test-analysis of two parallel). If the analysis is not to sea
Dual water sample relative deviation predetermined allowable value, as shown in Table 1 to perform.
4.7 sediments and organisms like double relative deviation table see GB 17378.5 and GB 17378.6.
4.8 natural samples spiked recoveries can not be beyond the range of values given method. Without this provision, executed in Table 2.
4.9 ocean monitoring, the use of analytical methods other than the specification must be done according to the provisions validation method comparison, reported to the competent authorities
Approval of the record.
Table 1 seawater parallel twin-like relative deviation table
The results where the magnitude 10-410-510-6 10-710-810-9 10-10
Relative deviation allowable limit /
1.0 2.5 510,203,050 calculation | AB | A + B × 100
Table 2 Recovery allowable value table
Concentration or amount range /
(Μg/L)
Recovery rate/
< 10 060 - 110
> 10 080 to 110
> 100 090 ~ 110
Capacity and weight method 95 - 105
5 Data Processing
5.1 significant digits and rounding off
5.1.1 significant figures
5.1.1.1 any specific measurement of the amount (given) Results are given by measuring the (fixed) value obtained was measured, also known as value. Measure
Usually a number multiplied by the unit of measurement used to indicate a specific amount of size. Unable to artificially achieve complete measurement (set) process, so
Measurement (fixed) result inevitably contain errors. In order to measure the expression (given) the accuracy of the results, with significant figures represents a specific measurement
(Be) the result of the digital section.
5.1.1.2 significant digits by one or more "reliable figures" and a "bottom owe quasi-digital" component. The effective number of significant digits is "
By the numbers "and" the last one due to quasi-digital "bits sum due under different specific measure (set) condition," bottom owe quasi-digital "level of under-registration
Different, so in principle, this standard does not perform rounding interval specified. But under normal circumstances, the analysis in the field of repair intervals about "the last
Less quasi-digital "1 unit.
5.1.1.3 The number of significant digits of significant figures, in addition to reflect the size of the magnitude of the field in the analysis also reflects accurately the value of
degree. For example 0.6705g sodium oxalate, the credible numerical values taken in the thousands on the 0 in the digital bit 5 is extremely suspicious,
Its true value lies between 0.6704g ~ 0.6706g.
5.1.1.4 significant digits "0" is calculated as the effective number of significant digits, according to the digital status "0" position before and after while
set. Common are the following four cases.
--- In the non "0", "0" numbers, such as between the two 2.005,1.025 three significant digits "0" should be counted as a valid number
The effective number of bits (referred to as the effective number of bits).
--- In the non "0" after the number of all "0" shall be calculated as the effective number of bits (All integers trailing "0" excluded). Such as 2.2500,
1.0250.
--- Front does not have a non-zero number "0", such as 0.0025 in the three "0" should not be counted as significant digits, only held in position. one
As it can be expressed as 2.5 × 10-3.
--- Integer behind the "0", it is difficult to determine whether a valid number. For example 1.5g may also be expressed as 1500mg, from the apparent point of view, with
A significant digits values are different. To avoid misunderstanding, unified with the index form, the above example can be written as 1.5 ×
103mg, shown to be two significant figures.
5.1.2 of the original recording data
To ensure the accuracy of the data should be, it should be properly recorded raw data begins, there is a calculation of significance for any data to be cautious
To assess properly documented significant digits magnitude. For example, the minimum scale 50mL burette is 0.1mL, and because a permit to increase
Bit estimates can be recorded to two decimal places, such as 12.34mL. This value indicates that 3 out of position on the scale indicates the value is exact to
Letter; 4 percentile is estimated on the interpretation, it is suspicious numbers, and knowing the fluctuation range 0.02mL, its relative error is (0.02 /
12.34) × 100% = 0.16%. If the original record is only recorded 12.3mL, said possible relative error of 1.6%. due to
Original records unreasonable resulting data accuracy decline an order of magnitude. But it can not arbitrarily increase the number of significant digits. As in the previous note to
12.340 is significant distortion, because it is impossible to estimate the two digits. Original record significant digits both essential, nor more.
Principle remembering that faithfully records and allow a write-up estimates are based on the minimum scale value Instrument indication.
General laboratory measuring instruments can remember bits as follows.
--- Millionth scale. 4 decimal places that is extremely bits.
--- Balance the dish. ie after the second decimal place percentile.
--- Spectrophotometer. absorbance third place that is charged to the thousandth decimal places.
--- Glass Container. remember significant digits shall be determined according to the allowable error and the gauge reading error.
First common gauge accurate recording capacity for recording in the format of Tables 3 and 4.
5.1.3 effective digital arithmetic rule
In order to ensure that the final results include only significant digits (position "0" exception), the effective number crunching to comply with the following rules.
--- Subtraction. the final calculation result decimal places reserved, should participate in the operation of the least significant digits of the decimal digits by
the same.
--- Multiplication and division operations. Operational Results after rounding, retain significant digits significant digits and should participate in operations in several significant figures
The same happened in person.
--- Logarithm. The number of significant digits and should the original number (real number) is the same.
--- Square, cube, square root. the results of significant digits should be the same and the original number.
Significant digits --- π, e 2 and Sang, Sang 3,13, etc., shall be decided with reference data associated with reserved places.
--- A set of data from a normal population, more than four, the number of significant digits than the increase in the average value of an original number.
--- For representation or analysis precision standard deviation, median effective figures generally take one; when measured more frequently
When two desirable, and you can only take two.
--- The report analyzes the results of significant digits, ie standard deviation should be determined according to the size of the precision analysis. Generally desirable quarter
The difference between a standard where the first few digits as mantissa analysis results. For example, a measurement result of 25.352, standard deviation
1.4, a quarter of a standard deviation of 0.35, which is the first digit where digit decile, the last one that is scheduled for the results may be reported as
25.4.
Table 3 First-free pipette accurate indexing capacity expressed in milliliters
Capacity indication allow accurate differential capacity
2 ± 0.006 2.00
3 ± 0.006 3.00
5 ± 0.01 5.00
10 ± 0.02 10.00
15 ± 0.03 15.00
20 ± 0.03 20.00
25 ± 0.04 25.00
50 ± 0.05 50.00
100 ± 0.08 100.0
Table 4 equal amounts into a flask formula accurate capacity expressed in milliliters
Capacity indication allow accurate differential capacity
10 ± 0.02 10.00
25 ± 0.03 25.00
50 ± 0.05 50.00
100 ± 0.10 100.0
200 ± 0.10 200.0
250 ± 0.10 250.0
500 ± 0.15 500.0
1000 ± 0.30 1000.0
2000 ± 0.50 2000.0
5.1.4 rounding off
Rounding off should observe the following rules (see the relevant provisions of GB 8170).
--- Discarded in the proposed figures, the first digit on the left if less than 5 (not including 5) When you lay down the last digit that is intended to be retained unchanged.
Example 1.
The 14.2432 rounded to one decimal place.
Before rounding after rounding
14.2432 14.2
--- Discarded in the proposed figures, if the first number on the left is greater than 5 (not including 5), then enter one of the last digit that is intended to be retained
plus one.
Example 2.
The only 26.4843 rounded to one decimal place.
Before rounding after rounding
26.4843 26.5
--- Discarded in the proposed figures, if left of the first number is equal to 5, the number on the right is not all "0", then enter a; if 5
On the right are "0", the last digit to be retained if you have an odd number is a forward, even if it is (including "0") will not enter.
Example 3.
The following values are rounded to one decimal place only.
Before rounding after rounding
0.3500 0.4
0.4500 0.4
1.0500 1.0
--- Abandon the proposed figure, if it is more than two figures can not be multiple consecutive rounding, figures should be based on the proposed discard the left
The first number of the size, according to the predetermined time rounding the result.
Example 4.
The 15.4546 rounding to an integer.
The correct approach is. before rounding after rounding
15.4546 15
Incorrect approach. once before rounding rounding rounding second
15.4546 15.455 15.46
Three four rounding rounding (result)
15.5 16
In rounding calculation process is not required for intermediate results about the final result rounded to the expected number of digits.
5.2 statistical test of outliers
One group (group) normal measurement data, should come from the same population with a certain distribution; if the analytical conditions change significantly, or in experiments
Operation fault occurs, will produce a significant difference with the normal data data, such data is called outliers or outliers. Outlier
Or outliers shall be tested to determine. The apparent difference in the larger analysis of data, but not tested or determined to be outliers abnormal value,
Called suspicious data.
5.2.1 Test suspicious data
Excluding outliers, the measurement result will be more objective; it should not be arbitrarily deleting some of the apparent differences between the larger and not stray suspicious data.
Suspicious data choice, should refer to the following principles.
--- Careful review process and review the generated test data is questionable, if it is the fault of the error, then discarded.
--- If you do not find fault, according to the statistical test procedures, decide whether to discard as outlier or outliers.
Criterion 5.2.2 outlier data
Discrimination outlier data should follow these guidelines.
--- Statistic calculated value is not greater than the significance level α = 0.05 threshold, the suspect data as normal data, should be retained.
--- Statistic calculated value is greater than the critical value α = 0.05 but not greater than the critical value α = 0.01, and this suspect data for the partial
From the data can be retained, taking the median instead of the average value.
--- Statistic calculated value is greater than the critical value α = 0.01, and this value is questionable outlier should be removed, and the remaining data continue
Test until the data is no exception value.
5.2.3 Test Method outliers
A set of measurement data consistency check and eliminate outlier test, as follows.
--- Repeated times like the measured values in ascending order of X1, X2, X3,, X-shaped;
--- Table 5 formula, find calculate Q value;
--- According to the selected significance level α and the number of repeated measurements like, look-up table 6 was critical value Qα;
--- Press Criterion 5.2.2, the decision to choose. If Q > Q0.01, the value of suspicious outliers discarded.
1) If Q0.05 < Q≤Q0.01, the offset value is questionable, can be retained, taking the median instead of the average value.
2) If Q≤Q0.05, the normal value of the suspicious reserved.
Example 5.
A set of measured values from small to large order for the 14.56,14.90,14.90,14.92,14.95,14.96,15.00,15.00,15.01,15. 02.
14.56 minimum test whether outliers.
The minimum value X1 suspicious when, according to equation (2) calculate statistics Q.
Q = X2-X1X like -1-X1
= = 14.90-14.5615.01-14.56
0.755 (2)
When state = 10, a significant level of α = 0.01, the critical value of 0.597 6 look-up table, because 0.755 > 0.597 ie Q > Q0.01, the minimum value X1 is determined to be abnormal, should be
Removed.
Shaped range dubious value is the minimum to the maximum ...
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