Directives for the work of reference materials (5) Technologic rules for reference materials of chemical composition
Some standard content:
URC CCG.3
National Standard of the People's Republic of China
CB/T 15000. 1---15000. 5--94 Directives for the work of reference materials
Promulgated on March 11, 1994
State Technical Supervision Bureau
Implementation on April 1, 1994
National Standard of the People's Republic of China
Directives for the work of reference materials (5)
Technical rules for reference materials of chemical composition
Directives for the work of reference materials (5)Technical rules for referehce materials pf chemical rompositian1Subject content and applicable scope
tH/T15000.5-94
This standard specifies the technical requirements for the preparation, evaluation and packaging of chemical composition standard samples of body, relative humidity and gas. This standard is applicable to the analysis of the chemical composition of solid, liquid and gaseous standard samples. 2 Referenced standards GB/T8171 Rules for rounding off values GB/T5274 Preparation of mixed gases for calibration of gas analysis GB/T5275 Preparation of mixed gases for calibration of gas analysis GB/T10245 Preparation of mixed gases for calibration of gas analysis Static emulsion method GB/T15003.2 Working guide for standard samples (2) Definition of common terms for standard samples GB/T15001.3 Working guide for standard samples (3) General rules and statistical methods for determining the value of standard samples GR/T15000.4 Working guide for standard samples (4) Provisions on the contents of the certificate for standard samples Part I Technical general introduction to standard samples for chemical composition of solids 3 Preparation 3.1 Selection of materials 3.1.1 The quality and properties of the standard samples should meet the expected requirements of the standard samples. For example, geological standard samples should be representative, and the materials used in the standard samples should not contain pores, cracks, and light defects.
3.1.2 When preparing standard samples for the basic products, the content of the main components should comply with the technical specifications of the product, and the impurity content should be higher than 30% of the upper limit.
3.1.3 The series of standard samples should reasonably arrange the gradient change of the performance coefficient values, so that the core standard samples can cover more product types. If necessary, the matrix or residual composition of each standard product should be as close as possible. 3.1.4 The selected materials must have enough quantity to ensure that they can meet the needs of use. 3.2 Material preparation 3.2.1 The process and preparation technology of the finished product should ensure the homogeneity of the finished product: avoid contamination of the container and the environment to the finished product, prevent direct contact with the particles, and pay attention to the loss of volatile components. State Technical Supervision Bureau 1994-D3-11 approved 1994-04-01 implementation CB/T15000.5--54 3.2.2 Process materials, especially those that are easy to be averaged, should be processed and averaged before processing, and the finished product should be recorded. In addition, the finished product should be physically inspected to ensure that there is no deficiency in the standard sample. 3.2.3 The sample composition and processing technology of the standard instrument such as photoelectric spectroscopy, photoelectric reading, X-ray fluorescence spectroscopy should be described. If other process conditions are also applied, experimental data should be attached. 3.2.4 Application characteristics of standard products: The properties of the selected materials should be selected. The material preparation should be in a suitable form, such as powder, crumbs, etc.
3.3 Separation of sodium materials
3.3.1 For the material used to prepare the standard product, several representative sampling points should be determined at its easily segregated parts, and samples should be selected for segregation test.
3.3.2 Add 1 powdered tablet of the standard sample to the material and divide it into four parts to make a suitable weight (for example, about 3.5 kg). 3.3.3 Segregation test 4.1 All samples must be subjected to uniformity test after preparation or after product preparation. 4.2 The purpose of the uniformity test is to determine whether the product is uniform or not. The method used for the uniformity test should be a method with high precision and should be at least equivalent to the specified method.
4.3 Representative and easy-to-analyze instruments should be selected for uniformity test. For standard products, the uniformity test should be carried out on all parts of the product and the method and quantity should be specified. 4.4 Randomly select a number of inspected products to reflect the overall characteristics of the samples. Under the condition that the conclusion is credible, a number of samples can be reduced, but not less than 15 (sets). When the total number of units is less than 1000, 1520 (sets) shall be selected; when it is greater than or equal to 10H, the number of samples selected shall be 2×10 (N is the total number of units).
Note: For samples with uneven quality (such as fast-moving products), increase the number of samples according to the actual situation, and conduct risk inspections one by one if necessary. 4.5 After the number of samples is confirmed, randomly select the samples to be inspected (see Appendix A or Appendix B): 4.E Use the following test method or the range test method for statistical inspection (see Appendix B for the critical value table of the F test method and Appendix C for the range test value table)
4.7 The series of standard samples should be inspected, and the standard products of the instrument should be randomly selected according to the variation of the standard samples. Take 5-10 sets at random, use the best analysis conditions, and draw the working curve. The effective point should fall on the working curve or close to the working curve. If there are individual points that are far from the working curve, the reason should be explained.
5 Value determination
-5..1 Only samples that have passed the uniformity test can be valued. Value determination can be carried out in one of the following ways. 5.1.1 Absolute measurement method,
5.1.2 Two or more accurate and reliable methods with the same principle are used to obtain collaborative values. These methods have been carefully studied and have a high degree of reliability.
5.1.3 More than 100 experimental results are collaboratively determined using accurate and reliable measurement methods with different principles. 5.1.3.1 The collaborative inspection room must be recognized by the state or department. If necessary, the inspection room must also be quality controlled and clear guidelines must be formulated.
5.1.3.2 The minimum number of independent measurement results obtained by the collaborative laboratory for several days or according to the specified method is generally not less than 8 groups, and each group reports independent data.
52 Processing of fixed value data
5.2.1 The fixed measurement data are processed according to the laboratory and the measurement method. After technically eliminating the suspicious values of the pulse cause, the Grubbs test method (see Appendix D for the critical value table) or the Jackson test method (see Appendix E for the critical value table) are used to statistically eliminate the suspicious values. If necessary, the original laboratory may be required to recheck the values. When the data are relatively sensitive or the range of possible values is large, the inspection should include the measurement method used by each laboratory, the measurement conditions and the operation process. When the source is confirmed, 5.2.2 All data shall be tested for normality. Under the condition that they obey the normal distribution or are approximately normal distribution, the mean value of the data obtained by each test and each flow determination method shall be regarded as a single measurement value to form a new set of measurement data. Calculate the mean value and standard deviation. 5.2.3 When determining that the accuracy and precision of the measurement data of one or more laboratories are comparable to those of several other laboratories, the unequal distribution method may also be adopted, using the weighted mean value and the corresponding standard deviation as the standard value and standard deviation. 5.3 Representation of measurement results
5.3.1 Rounding off of numerical values It shall be carried out in accordance with the provisions of GH/T8170 standard. The measured deviation shall be approximated according to the lower limit, and its digits shall be aligned with the digits of the standard value. 1 to 2 valid mathematical values shall be retained. 5.3.2 The result of the fixed value shall be expressed as standard value and uncertainty. 6 Stability test
6.1 The marked product shall be regularly tested for stability under the specified conditions. When there are multiple performance indicators, the performance parameters with variable characteristics can be selected for inspection and adjustment:
6.2 Qualitative test can be carried out according to the determination method of fixed value. 6.3 When the deviation of the measured results in different time intervals and the standard value does not tend When the precision of the test method is passed, the stability of the standard sample is considered to meet the requirements.
6.4 Standard products should have a clear validity period. ? Packaging
7.1 Standard products should have a specified qualified packaging format to facilitate transportation and long-term storage. 7.2 Each packaging unit should have a standard product label and a standard sample certificate. 7.3 For products that require special storage conditions to ensure stability, indicate and use the standard seal.
Technical Specifications for Standard Samples of Liquid Chemical Components B Preparation
8.1. Material Preparation
B.1.1. The materials for preparing standard samples can be directly collected from representative natural materials. After processing, their properties should meet the expected requirements of standard samples.
Pure substances with standards or criteria should be selected and prepared according to the specified characteristics and technical conditions. The standard samples should have representativeness and compatibility, and their properties and compatibility should also meet the expected requirements of standard samples. 8.1.2 The selected material group (or sample system) should meet the technical requirements specified in the reference standard and standard analysis method. 8.1.3 The basic composition property values of the selected material group should be representative and comparable. The number of standard samples cut should be sufficient to ensure that the actual needs are met.
8.2 Material processing
8.2.1 For the natural materials collected, the appropriate processing technology and appropriate storage conditions should be selected according to the properties of the selected materials to maintain the homogeneity and stability of the standard samples. When using the reference or standard pure substances as materials, the appropriate processing technology and appropriate storage conditions should also be selected according to the properties of the materials and the basic composition and performance value of the prepared standard samples to maintain the expected homogeneity and stability of the standard samples.
B.2.2 No foreign matter should be mixed into the material during the material processing. 8.2.3 For the particles that are difficult to be homogeneous, the homogeneity should be initially checked during the processing. 8.2.4 After the material is processed, it should be divided into the smallest packaging. 21
9 Homogeneity test
GB/T15000.5-94
9.1 For the samples that have been prepared and initially homogenized, after being divided into small packaging units, the F test method (for the table of threshold values, see Appendix B) and the T test method (see Appendix F>) shall be used for homogeneity test. 9.2 The unit efficiency of the product and the number of repeated measurements of each sample shall meet the requirements of statistical test. When the number of samples is 15~25 or more than 1000 packaging units, the number of samples shall not be less than 31. After the number of samples is determined, the samples shall be randomly selected.
9.3 The components with representativeness and difficulty in uniformity shall be selected for uniformity test. The minimum number of repeated measurements for each sample shall be not less than 13 times. 9. 4. The quality test should be carried out by a high-precision determination method: The determination of the same performance value should be carried out by the same operator and the test equipment and instrument status should be checked to ensure consistency. 10 Determination of value
10.1 Determination method The sample that is used for the quality test can be determined in the following ways. 10.1.1 Absolute measurement method
10.1.2 Accurate and reliable methods based on two or more different principles. 10.1.3 Collaborative determination by multiple laboratories using accurate and reliable methods. 10.1.3.1 The collaborative laboratory selected by the product development unit must have a high level of testing. When necessary, it shall conduct a joint control of the operating laboratory and formulate clear guidelines. 10.1.3.2 The minimum number of independent test results reported by the participating laboratories on a daily basis or according to the test method shall generally not be less than 8 Groups, each group reports no less than 6 drug data, 10.2 Processing of fixed value data
10.2.1 For each laboratory or each test method, 6 independent data are batched out. After technically eliminating the suspicious values with clear reasons, use the Glass test method (Glass critical value table Appendix D) or the Johnson test method (Glass test method critical value table Appendix E) to statistically eliminate the suspicious values. If necessary, it is required to conduct a test on the suspicious values. When the data are relatively complete or there are many suspicious values, the test methods, measurement conditions and operating procedures used in each laboratory should be carefully checked. 102.2 All data should be tested for normality of distribution. If the results are abnormal, it can be judged by observing the histogram or using the GB4882 normality test method, or collecting relevant test experience to determine whether it is abnormal. Normal distribution. If the data are relatively scattered and the distribution is multi-peaked, the laboratory should carefully check the laboratory's determination conditions, measurement conditions and operation process. Find out the reasons and make improvements, and then re-measure. 10.2.3 Under the condition that the data obeys normal distribution or approximate normal distribution, the average value of each test data of each test method of each experiment is defined as a single determination value, forming a new set of data, and calculating its mean value and standard deviation. 10.2.4 When the stability is poor and there are many test batches, the median value and the uncertainty of the median value can also be used as the standard value and uncertainty. 10.3 Presentation of determination results 10.3.1 The numerical value is determined in accordance with the provisions of GB/8171; the standard deviation is determined by the standard deviation, and its digits are aligned with the standard elimination number: generally 1 to 2 significant figures are guaranteed. 10.3.2 The determination results are presented as standard values and uncertainties. 11.1 The stability test of the standard sample should be carried out regularly under the specified storage conditions. When the standard sample has multiple performance values, the variable and representative performance values can be selected for testing. 11.2 The stability test method can be carried out according to the fixed value determination method. 22
GB/T 15000.5—94
11.3 When the accuracy of the results of the determination does not exceed the precision of the test method, the sample is considered to be accurate within the test time. The standard sample is effective. 12 Packaging, storage and transportation
12.1 The non-standard product should be placed in a container with different properties: the standard sample with corrosion resistance should be packed in a strict packaging,
12.2 The packaging container should have the standard sample mark, etc., and the standard sample certificate should be provided. 12.3 For the convenience of use, standard samples can be packaged in different units according to different varieties and requirements: 12.4 The marked samples should meet the requirements of the products and storage methods. For the storage, analysis and transportation with special requirements, clear regulations should be made. Part III
Technical Specifications for Standard Samples of Gas Chemical Composition 13 Names of Standard Samples of Gas Chemical Composition
The names of standard samples of gas chemical composition should be in the following format. 8. The name format of the specified component is "*×× Standard Sample of Gas Chemical Composition", such as: "Gas Chemical Composition Standard Sample of Carbon Dioxide".
1. The name format indicating the purpose is "gas chemical composition standard sample for ××", for example, "gas chemical composition standard sample for carbon dioxide analyzer",
; the name format indicating the preparation method is "×> gas chemical composition standard sample, for example: "high temperature hydrogen peroxide gas chemical composition standard sample",
14 Expression of component quantity
14.1 The component quantity of the gas chemical composition standard sample is generally expressed in degrees. The concentration unit should preferably be one of the following three: molar ratio, liquid concentration, ×× million (mal/mol>, ×× mole/mal, mass concentration, ××% (m/m), ××g/g
volume of liquid 14.2 The amount of the components of the standard sample is expressed in terms of permeability, and the unit is min. 14.3 The concentration of the gas chemical composition standard product is called the gas chemical composition standard sample with a concentration of 1% (V/V); it is called the trace gas chemical composition standard sample when it is below 0.1% (V/V). 15 Technical requirements
The technical requirements for gas chemical composition standard samples should include the following contents. Standard value (or range)
Uncertainty
Specified period;
High filling pressure (for commercial pressure standard samples): Minimum usable pressure (for high pressure standard samples) ): Use temperature (do not penetrate into the standard sample). 16.1 Raw materials 4 16.1.1 The raw gas used to prepare the standard sample of gas chemical composition must have a quality certificate or analysis report. 23 16.1.2 When preparing the standard sample of gas chemical composition, the raw gas must have a quality certificate or analysis report. 23 16.1.3 When preparing the standard sample of gas chemical composition by weight method, the analysis of various impurities in the raw gas must meet the requirements of the determination, and the analysis report with high accuracy should be used. Method. 16.2 Containers
162.1 The containers for gas chemical composition standard samples can be made of aluminum, steel, and other materials. The latter two are made of aluminum, and the chemical composition standard products of micro-organisms or chemically active micro-organisms must be contained in aluminum bottles. 16.2.2 Steel bottles, alloy bottles, glass bottles, and calcium bottles: they must be inspected in accordance with relevant regulations! Appearance inspection. 16.2.3 The outer surface of the high-pressure container should have a mark showing different types of gases. Different gases and high-pressure containers are not allowed to be mixed. 16.2.4 The high-pressure container should be heated and air-conditioned before use. The residual moisture in the container of the gas chemical composition standard product should be less than 1rL/1..5.16.3 Preparation of gas chemical composition standard samples 16.3.1 Gas chemical composition standard samples are prepared individually. 16.3.2 When using the cupping method, the method should be carried out in accordance with GB/5274. The weighing method is currently the most accurate method, and its uncertainty in the value can reach 0.1% to 1%. Therefore, the most accurate method should be selected first to prepare gas chemical composition standard samples. 16.3.3 When using the permeation method, GB3/T527: should be followed. 16.3.4 When using the state volume method, GB/T10245 should be followed. 16.3.5 When using the pressure method, flow method, and method, etc., the relevant specifications should be consulted. 17 Homogenization treatment After preparation, the container containing the gas chemical filtration standard sample must be subjected to a frequency of more than 30mil (or rotation) treatment. 18 Determination
18.1 The determination of gas chemical composition standard samples is generally completed by one laboratory. When the determination is jointly carried out by several laboratories, the numerical processing shall be carried out in accordance with GB/15000,3.
18.2 The gas chemical composition standard samples prepared by the weighing method shall be preferably used as the basis for the determination of gas chemical composition standard samples prepared by other methods.
183 The determination of difficult samples shall be carried out by gas analysis of equivalent quality. 18.4 When determining the value, the uncertainty of various factors affecting the accuracy of the determination shall be calculated one by one and all shall meet the technical requirements. 19 Comparative analysis
19.1 After the determination of the gas chemical composition standard samples, one or more methods shall be used to make comparative analysis. The data obtained by the comparative method shall not be less than four.
19.2 When the uncertainty of the comparative analysis method is significantly better than the uncertainty of the fixed value, the comparative error limit is equal to the uncertainty of the fixed value. When the uncertainty of the inverse analysis method is equivalent to or slightly different from the uncertainty of the fixed value, the comparative error limit should be equal to the sum of the two. If multiple methods are used for comparative analysis, the uncertainty of different methods should be obtained and the comparative difference should be calculated separately. 19.3 When the difference between the comparative analysis value and the standard value is within the range of the comparative error tree, the test fixed value result is valid and the value should be re-determined. 20 Accuracy report
Each gas chemical component standard sample should provide more than 11 fixed value data. When the nominal value of the gas chemical component standard sample reported is a base, there should be at least two standards in the accuracy report that are respectively at the upper and lower limits of the range. 24
GI/T150D0.5:94
The gas chemical composition standard sample in the production report must be prepared by a certain method, but the original gas used may not be the same as the original gas used. The operator may also be a different person in the laboratory. 21 Stability test
21.1 Time stability test
When the gas chemical composition standard sample is developed or the process is changed, it must be tested and adjusted to determine the overall quality of its chemical composition. 21.1.1 Test method
Use the same method to analyze the chemical composition standard sample of the same unit regularly. The analysis method should have good reproducibility. The analysis time should be greater than 1/5 of the predetermined validity period. 21.1.2 Result judgment
The standard value is taken as the standard. When the difference between the analysis value and the standard value each time is not greater than the current uncertainty, the predetermined validity period is considered to be correct.
If the phenomenon of overpressure occurs, find out the reason. When it is confirmed that the error is not accidental, the predetermined validity period should be shortened. 21.2 Stability
When the standard sample of high-pressure gas chemical composition is developed or the process is changed, it must be subjected to a decompression test to determine the influence of pressure change on chemical composition.
21.2.1 Test method
Use the same supply: a standard sample of gas chemical composition, and analyze it under different pressures. The analysis method should have good reproducibility:
The change of pressure of the standard sample of gas chemical composition should be 1/10~1/5 of the difference between the given maximum filling pressure and the predetermined minimum usable pressure.
21.2.2 Result judgment bZxz.net
If the difference between the standard value and the standard value each time is not greater than the specified tolerance, it is considered that the predetermined amount is correct.
If the deviation is caused by pressure drop, the minimum available pressure should be increased. 21.3 The amount of the gas chemical composition standard sample put into the stability test should be no less than 2/3 of the prepared amount. 21.4 The above two tests can be combined. 22 Packaging, transportation and storage
22.1 The packaging container of the gas chemical composition standard sample should be labeled and certified. 22.2 The transportation of gas cylinders is recommended to comply with relevant regulations. 22.3 Gas chemical composition standard samples should be stored in an environment with an ambient temperature of 5-40°C, a relative humidity not exceeding 85°C, no sunlight, good ventilation, and a certain degree of safety protection. 25
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01 32 90 76 34||tt| |43 14 52 5 94
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55 34 2447 89
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61 29 08 93 67
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52 83 9c 94 76
16 55 23 42 45
B1 76 9 26 92
5535237918||tt| |16 45 70 50 83
KD 60 4718 7
82 95 55 26 5
63 14 2 32 52
86 53 E9 X 22
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89 64 58 69 75
79 24 166
03 73 52 16 56
35 21 20 71 34||tt| |33 92 74 65 94
80 53 54 7 27
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82 B8 33 69 95||tt| |4 0 8: 30 27
44 9114 66 47
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58 02 39 37 67||tt ||1B 74 72 00 1B
24 35 59 87 8
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OB 22 23 71 T7
GR/ T 15000.5-94
F513 car 78
$9 29 76 39 81
83 85 52 27 99
21 48 94 06 $3
60 55 55 00 27
62 33 74 62 14
40 14 71 4 53
95 94 78 32 65
64 B5 4 135 72
29 54 96 5384
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50 95 52 74 33
01 32 90 76 34||tt| |43 14 52 5 94
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55 34 2447 89
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61 29 08 93 67
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16 55 23 42 45
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KD 60 4718 7
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89 64 58 69 75
79 24 166
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80 53 54 7 27
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44 9114 66 47
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37 79 81 b3 74
58 02 39 37 67||tt ||1B 74 72 00 1B
24 35 59 87 8
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2B 45 82 58 72
OB 22 23 71 T7
GR/ T 15000.5-94
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$9 29 76 39 81
83 85 52 27 99
21 48 94 06 $3
60 55 55 00 27
62 33 74 62 14
40 14 71 4 53
95 94 78 32 65
64 B5 4 135 72
29 54 96 5384
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K2 07 5$ 89 35
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50 95 52 74 33
01 32 90 76 34||tt| |43 14 52 5 94
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KD 60 4718 7
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60 55 55 00 27
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$9 29 76 39 81
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60 55 55 00 27
62 33 74 62 14
40 14 71 4 53
95 94 78 32 65
64 B5 4 135 72
29 54 96 5384
93 075472 59
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3 39 3 05 33
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8 14 8 99 70
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16 55 23 42 45
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229129.6192191919||tt ||(100=)
contained* 99 -5 2
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