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The Production of Reference Materials for Geoanalysis
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JJF 1646-2017
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Basic data Standard ID | JJF 1646-2017 (JJF1646-2017) | Description (Translated English) | The Production of Reference Materials for Geoanalysis | Sector / Industry | Metrology & Measurement Industry Standard | Classification of Chinese Standard | A50 | Word Count Estimation | 17,167 | Date of Issue | 2017-09-26 | Date of Implementation | 2017-12-26 | Regulation (derived from) | General Administration of State Quality Inspection Announcement 2017 No. 78 | Issuing agency(ies) | State Administration for Market Regulation |
JJF 1646-2017: The Production of Reference Materials for Geoanalysis---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
(Technical specification for the development of standard materials for geological analysis)
People's Republic of China National Measurement Specifications
Development of Geological Analysis Reference Materials
The Production of Reference Materials for Geoanalysis
2017-09-26 Posted
2017-12-26 Implementation
General Administration of Quality Supervision, Inspection and Quarantine released
Development of Geological Analysis Reference Materials
Focal point. National Standard Material Measurement Technical Committee
The main drafting unit. National Geological Experimental Testing Center
Participate in the drafting unit. Hubei Province Geological Experimental Testing Center
Institute of Geophysical and Geochemical Exploration, Chinese Academy of Geological Sciences
This specification entrusts the national standard material measurement technical committee to be responsible for explaining
The main drafters of this specification.
Xu Chunxue (National Geological Experimental Testing Center)
Wang Yaping (National Geological Experimental Testing Center)
Participate in the drafters.
Fang Jindong (Hubei Geological Experimental Testing Center)
Wang Su Ming (National Geological Experimental Testing Center)
Gu Tiexin (Institute of Geophysical and Geochemical Exploration, Chinese Academy of Geological Sciences)
An Ziyi (National Geological Experimental Testing Center)
Sun Dezhong (National Geological Experimental Testing Center)
table of Contents
Introduction (Ⅲ)
1 Scope (1)
2 References (1)
3 Overview (1)
4 mining and preparation (1)
4.1 Candidate selection (1)
4.2 Candidate Preparation (2)
5 Uniformity assessment (2)
5.1 General requirements (2)
5.2 Features to be tested (3)
5.3 Sample Extraction (3)
5.4 Measurement and Analysis (3)
5.5 Minimum Sampling (4)
5.6 Data Results Statistics (4)
6 Stability Assessment (4)
6.1 General requirements (4)
6.2 test feature selection (4)
6.3 Sample Extraction (5)
6.4 Measurement and Analysis (5)
6.5 Inspection time (5)
6.6 Data Results Statistics (5)
6.7 Stability Monitoring (5)
7 setting (6)
7.1 General requirements (6)
7.2 Establishment and Proof of Metrology Traceability (6)
7.3 Cooperation Laboratory Requirements (6)
7.4 Setting method (6)
7.5 Measurement data validation and determination of value (7)
8 Evaluation of Uncertainty (7)
9 result of the rating (7)
9.1 Setting result representation (7)
9.2 revised value of about (8)
9.3 Amendments (8)
10 Packaging and storage (8)
10.1 Packaging (8)
10.2 Storage (8)
11 Development Report (8)
12 Certification (9)
Appendix A Preparation Examples of Solid Candidates (10)
Introduction
A wide range of geological materials, complex composition, almost all elements involved in the natural existence, its content span, points
The evaluation of the results strongly depends on the standard substance. Traceability of Establishing Experimental Measurement Results by Geological Analysis Reference Materials
To ensure the comparability of measurement results in different regions and at different times and to achieve the international mutual recognition of measurement results
effect.
This specification describes the development of geological analysis of the candidate material selection process and preparation, uniformity assessment,
Stability assessment, valuation, assessment of uncertainty, valuation results, packaging and storage, development reports and certificates
This principle and requirements, in order to regulate the development of China's geological analysis of the standard material to enhance China's geological analysis of the standard material
The quality level.
This specification is based on JJF 1342 "General Requirements for Development (Production) of Reference Materials", JJF 1343 "Standard
General principles of qualitative and quantitative principles and statistical principles "and JJF 1218" standard material preparation report preparation rules ", combined with
Qualitative analysis of the characteristics of the standard material. When using this specification, the relevant specifications above should be implemented at the same time.
This specification was first formulated.
Development of Geological Analysis Reference Materials
1 Scope
This standard specifies the geological analysis of the selection and preparation of standard materials, uniformity assessment, stability assessment, valuation,
Uncertainty assessment, valuation results, packaging and storage, research reports and certification requirements.
This standard applies to the development of geological analysis of the standard material, but also for geological analysis of quality control sample development
for reference.
2 reference documents
JJF 1006-1994 a standard technical specification
JJF 1059.1 Evaluation and Expression of Measurement Uncertainty
JJF 1071 National Metrology Calibration Code Writing Rules
JJF 1186 standard substance certification certificate and label content writing rules
JJF 1218 standard substance development report writing rules
JJF 1342 standard material development (production) agency general requirements
General Principles and Statistical Principles of JJF 1343 Standard Substance Setting
For dated references, only the dated version applies to this specification; for undated references
The latest version (including all amendments) applies to this specification.
3 Overview
3.1 Geological analysis of standard substances should be carried out before the development of planning work to determine the desired goal.
Note Expected goals include the characteristics of the reference material, substrate, quantity, and target measurement uncertainty.
3.2 Geological analysis of the standard substance uniformity, stability and the characteristics of the range of values should be suitable for the standard substance
the use of.
3.3 Geological analysis The standard substance should be of sufficient quantity to meet the needs of its use within the validity period.
3.4 series of standard material characteristics of the distribution of the value of the gradient should be as much as possible to meet the requirements of the use of less variety cover
The scope of the period.
4 mining and preparation
4.1 candidate election mining
4.1.1 General requirements
4.1.1.1 The selection of candidates should meet the applicability, representativeness, and easy-to-copy principle.
4.1.1.2 Candidates Generally, samples of natural state should be collected as candidates. Under special circumstances, if the natural state
Samples can not meet the needs of the actual research, but also by mixing, adding, etc. Preparation of candidates.
4.1.2 determine the sampling location
4.1.2.1 Candidates should first conduct data research and literature search prior to collection to grasp the basic information of candidates, including
The regional distribution of candidates, rock and mineral types, the content of the main measured indicators and so on. According to the plan's expectations
Target, initial screening sampling location.
4.1.2.2 site survey at the sampling point, collecting a small amount of samples. Through a small amount of sample analysis and testing, master
The main test characteristics of the value. If necessary, mineral composition analysis can be identified.
4.1.2.3 comprehensive information on the situation and a small amount of analysis of the sample to determine the candidate collection location.
4.1.3 collect candidates
4.1.3.1 Depending on the type of candidate, choose the appropriate method to collect the candidate.
4.1.3.2 The number of candidates collected should be greater than the expected number of preparations.
4.1.3.3 The candidate should be packed and transported to prevent damage, pollution and deterioration.
4.2 candidate preparation
4.2.1 General requirements
4.2.1.1 According to the nature of the candidate, choose a reasonable processing procedures, preparation process.
4.2.1.2 Candidates should be prepared to ensure uniform samples, as far as possible to avoid contamination and prevent the measured characteristics of the value changes.
4.2.1.3 Candidates should be prepared according to the different conditions of the material before preparation.
4.2.2 Preparation of solid candidates
4.2.2.1 The preparation of solid candidates are generally divided into five steps. drying, crushing, grinding, mixing, packaging and other five steps.
4.2.2.2 Single mineral candidates should be identified in the rock and mine after the general steps of preparation, mineral products candidate should be based on
Need to be selected in different stages after the general preparation steps.
4.2.2.3 Preparation of candidate particle size should meet the requirements of the test method for the sample size. If the standard material by the granularity shadow
Sound, solid candidates should be prepared after the particle size analysis to determine the candidate processing particle size distribution.
4.2.2.4 Preparation of solid candidates Particle size generally requires over 0.074 mm sieve (-200 mesh) over 98%.
Notes 1. Geological Analysis Standard Materials Solid candidates generally refer to rocks, ores, soils and sediments.
Note 2. When the candidate is easily water-absorbent and bonded, it is advisable to prepare a sufficiently dry sample while hot.
Note 3. See Appendix A for an example of the preparation of a solid candidate.
4.2.3 Preparation of liquid candidates
4.2.3.1 Preparation of liquid candidates are generally divided into filtration, mixing, packaging and other steps. When necessary, optional after dispensing
Select cobalt -60 (60Co) irradiation sterilization or infrared sterilization.
4.2.3.2 Need to add protective agent or stabilizer of liquid candidates should meet the requirements of the relevant standards.
Note. Geological Analysis Standard Materials Liquid candidates generally refer to groundwater.
5 Uniformity assessment
5.1 General requirements
5.1.1 Geological analysis The development of reference materials should be assessed for uniformity.
5.1.2 Uniformity assessment should be designed before carrying out uniformity assessment. Program should be clear characteristics to be tested, sampling
Product method, measurement and analysis methods, statistical methods and so on.
5.1.3 Geological analysis The characteristic value of the standard substance should be uniform. Although other properties of a standard substance may not
But as long as this nonuniformity does not have a detectable effect on the value of the property being measured, it can be assumed that the reference material
Evenly.
5.2 test characteristics of choice
5.2.1 In principle, the homogeneity should be evaluated for each test characteristic of the standard substance.
5.2.2 for a variety of standard materials, when it is difficult to test the uniformity of all properties should be based on
To be tested characteristics of the concentration range and the elements of the geochemical classification, choose a representative, not uniform characteristics of uniform
Sexual assessment, at the same time, must ensure that the untested characteristics of the uniformity in the same controlled state.
NOTE The properties to be measured without uniformity test may be based on the characteristics of their concentration and elemental properties in reference to the properties that have been tested for uniformity
Enter the uncertainty of the assessment.
5.2.3 If the number of features to be tested is M, select the number of characteristics to be evaluated for uniformity, p,
The number of sexual should meet the following requirements. When M ≤ 15, p = M; \u003cM ≤45时,15≤p≤M ;当
When M > 45,
3M ≤p≤M
5.3 Sample Extraction
5.3.1 Extraction method
5.3.1.1 Uniformity assessment should generally be taken after the standard substance is subdivided into the smallest packing units. If the standard substance
A large number can not be completed in a short period of packing, samples can be randomly selected in the sample, but the sample should be distributed in
The entire process of discharge, and re-inspection after the sample packaging.
5.3.1.2 If the standard substance is not easy uniform, in the preparation process should be randomly selected samples for homogeneity of the initial test, pass
After packing into small packaging unit.
5.3.2 Number of extraction units
5.3.2.1 The number of extraction units should be adequately representative of the total number of reference materials.
5.3.2.2 The number of extraction units depends on the number of units of the total sample, and the number of extraction units and the repetition of each sample
The number of measurements should be suitable for the statistical test used.
5.3.2.3 If the total number of elements is N and the number of extraction units is q, the number of extraction units shall meet the following requirements.
When N ≤200, q≥11; when.200 \u003cN≤500时,q≥15;当500\u003cN≤1000时,q≥25;当
When N > 1000, q ≧ 3 ·
3N. For samples with good uniformity, q≥10 when N≤500; when N > 500
When q ≥ 15. The corresponding relationship between the number of extracted units and the total number of units is shown in Table 1.
Table 1 the number of extracted units and the overall number of units of correspondence
Total number of units N Extraction unit number q
N ≤.200 q ≥ 11
200 \u003cN ≤500 q≥15
500 \u003cN ≤1000 q≥25
N > 1000 q ≧ 3 ·
Good uniformity of the sample N ≤ 500 q ≥ 10
Good uniformity of the sample N > 500 q ≥ 15
5.4 Measurement and Analysis
5.4.1 The general should choose not less than the precision of the method of setting, with sufficient sensitivity measurement method.
5.4.2 Sample Weighing quality depends on the measurement method and candidate processing grain size.
5.4.3 Under normal circumstances, each extraction unit should be independent sampling repeated measurements ≥ 2 times.
5.4.4 Uniformity assessment is usually carried out in a random order.
Note. Measuring in a random order prevents time variation in the measurement system (drifts during measurement) from interfering with uniformity assessment.
This can be done by randomizing the sample vial sequence while changing the sample measurement sequence. For example, assume 10 samples
To assess the uniformity, do 3 repeated measurements, measurement programs can be as follows.
Repeated measurements 1.1-3-5-7-9-2-4-6-8-10;
Repeat measurement 2.10-9-8-7-6-5-4-3-2-1;
Repeat measurement 3.2-4-6-8-10-1-3-5-7-9.
5.4.5 All measurement and analysis results should be involved in the uniformity assessment data processing.
5.5 Minimum sampling volume
5.5.1 Geological Analysis After the uniformity of reference material is assessed, the minimum sample size to be applied shall be given.
5.5.2 Geological Analysis The minimum sample size for a standard substance is usually the standard used in the homogeneity assessment measurement analysis
Quality of the quality. When there is more than one characteristic value to be measured, the standard should be expressed in the minimum sampling amount of the characteristic to be tested that is not easily uniform
The minimum sampling amount of quality or the minimum sampling amount for each characteristic to be measured.
5.5.3 Geological Analysis The minimum sample volume of a standard substance can also be experimentally determined. Pass different sample volume conditions
The obtained standard deviation of the bottle and the sample volume to determine the minimum sampling volume.
5.6 Data Results Statistics
The results of the uniformity assessment of the data should be consistent with the results of JJF 1343 "standard principle of value of the general principles and statistics
Reason "requirement.
Note 1. Geological analysis of the uniformity of the standard material assessment, in most cases the use of univariate analysis of variance for uniformity assessment.
In some cases, two-way ANOVA can also be used to assess uniformity.
Note 2. Although other types of statistical methods (eg, mean consistency test, t test, range method, etc.) are also available
It is used to evaluate the uniformity of reference materials for geological analysis, but this standard does not cover this aspect.
6 Stability Assessment
6.1 General requirements
6.1.1 Geological Analysis Stability assessment should be carried out during the development of reference materials, generally after the assessment of homogeneity.
6.1.2 Stability assessment should be designed before the stability assessment program, the program should be clear shipping conditions, saving
Pieces, test features, sample extraction methods, measurement and analysis methods, test time points, statistical methods and so on.
Note.Transport conditions should be optimized as much as possible to ensure that the instability of standard substances during transportation does not exceed the instability
Sex. When the impact of transport conditions on the stability of standard substances exceeds the impact of storage conditions, should consider the short-term stability of the right
The contribution of the degree of certainty.
6.1.3 Geological analysis of the standard material should be under definite conditions, in a longer period of time to be tested steady characteristics
Qualitative assessment.
6.1.4 When necessary, should be simulated by transport and harsh conditions of temperature, place of inspection and other reference material in special
Short-term stability under certain conditions.
6.2 test feature selection
6.2.1 In principle, the stability of each of the test substances to be tested shall be evaluated.
6.2.2 for a variety of characteristics of the standard material, when it is difficult to test the stability of all properties should be based on
Concentration range and geochemical classification of characteristics to be tested, the choice of representative, not easy to be stable characteristics of stability assessment
Estimated, at the same time must ensure that the stability of the unschecked features in the same controlled state.
Note. The characteristics to be tested that have not been subjected to the stability test may be based on their concentration and elemental properties, referring to the characteristics that have been subjected to the stability test
Enter the uncertainty of the assessment.
6.2.3 If the number of characteristics to be measured is M, the number of characteristics chosen for stability assessment is r, and when M ≤ 15
When r = M; when 15 \u003cM ≤45时,15≤r≤M ;当M \u003e 45 hours,
3M ≤ r ≤ M
6.3 Sample Extraction
6.3.1 The assessment of stability should normally be taken at random after the reference material is dispensed into the smallest packing unit.
6.3.2 Extraction Sample unit distribution should be adequate for the overall sample.
Note. To reduce the effects of standard material inhomogeneities, multiple determinations can be performed on a single sample, which gives better results than a small sample
Complex test. That is, when the stability of the measurement of the standard deviation of reproducibility and uniformity assessment and standardization of the value of the standard repeat
When there is comparability of the quasi-deviations, it is possible to reduce inhomogeneities at each measurement by sampling multiple bottles at each time point
influences.
6.4 Measurement and Analysis
6.4.1 generally should not be less than the method of choice of precision and sensitivity with adequate measurement methods.
6.4.2 Evaluation of the stability of different test points, steps and experimental conditions should be consistent.
6.4.3 Repeat the measurement of each standard material should be ≥ 2 times.
6.4.4 All measurement and analysis results should be involved in the stability assessment data processing.
6.5 test time
6.5.1 Short-term stability assessment The inspection cycle is usually short but at least as long as the transport of the reference material.
Short-term stability assessment, the general choice of time points ≥ 3 months.
6.5.2 Long-term stability considerations Period should be ≥12 months, the general choice of time points ≥5.
6.6 Data Results Statistics
6.6.1 The results of the stability assessment The statistics should be consistent with JJF 1343 "General principles and statistics of the value of the standard substance
Principles of learning "requirements.
6.6.2 The validity period of national standard substance should generally be over 1 year. The effective period of national secondary standard substance should be
In more than six months.
6.6.3 The determination of the validity period of reference substance can also be given with reference to the expiry date of a similar reference standard substance.
6.7 Stability Monitoring
6.7.1 Periodicity should be checked regularly during the use of standard substances to ensure that the published value is accurate and reliable.
6.7.2 The stability of the reference material can be monitored using equation (1).
xCRM-xmeas ≤ k u2CRM u2meas (1)
In the formula.
xCRM --- Certified value of the standard substance;
xmeas --- measured value;
uCRM --- standard material synthesis standard uncertainty;
umeas --- standard uncertainty of stability monitoring measurement results;
k --- confidence probability of 95% obtained when the appropriate inclusion factor.
If the condition of formula (1) is satisfied, the standard substance is stable enough.
7 fixed value
7.1 General requirements
7.1.1 Geological analysis The certified value of the standard substance should be traceable to SI units or reference standards as far as possible.
7.1.2 Before setting the value, the developer shall formulate the operation guideline for setting value of reference material, including the expected identification of reference material
Value range, processing and preparation and uniformity assessment, etc., and to develop concise guidelines su...
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