HG 2955-1989 Rules for the preparation of standards for molecular absorption spectroscopy analysis methods
Some standard content:
UDC 543.422.5/.6
National Standard of the People's Republic of China
GB 10713--89
Adjusted to; HG hzgrs-8
Rules for drafting molecular absorptionspectrometry analysis standards1989-03-31issued
198912-01implemented
issued by the State Bureau of Technical Supervision
Subject content and scope of application,
2 Referenced standards
3 Terminology
4 Basic requirements for the preparation of molecular absorption spectrometry analysis methods standards 5
Constitution of molecular absorption spectrometry analysis methods standards Overview part
Main body
Supplementary part
National standard of the People's Republic of China
Molecular absorption spectrometry analysis methods standards
Rules for drafting molecular absorption spectrometry analysis standards This standard refers to the international standard ISO78/3-1983 "Chemical-Spectrometry Analysis Method Standard".
1 Subject content and scope of application
Standard format I
GB 10713--89
I Part III: Molecular absorption
This standard specifies the general composition, content and requirements for the preparation of standards for molecular absorption spectral analysis methods for solutions tested in the visible light region and near ultraviolet light region.
This standard is applicable to the preparation of national standards and professional standards (departmental standards) for molecular absorption spectral analysis methods, and should also be used as a reference when preparing local standards and enterprise standards for molecular absorption spectral analysis methods. Reference standards
GB 1.1 Guidelines for standardization work Basic provisions for standard writing GB.1.4 Guidelines for standardization.L work Standard provisions for chemical analysis methods GB8322 Molecular absorption spectroscopy Terminology
3 Terminology
3.1 Laboratory sample laboratorysample Sample prepared for inspection and testing in the laboratory 3.2 Test sample
A sample prepared from a laboratory sample according to certain requirements, and the test material is obtained from it. 3.3 Test material test portian
A certain amount of sample weighed for inspection or observation (if the sample and the laboratory sample are the same, the laboratory sample is weighed).
3.4 Standard solutionstandard solution A solution that accurately determines the concentration of a certain element, ion, compound or radical. The concentrations of these solutions are expressed in mo1/L (or g/L) or their fractions or multiples.
3.5 Set of calibration solution A series of standard solutions of different concentrations of the test component prepared for drawing the calibration curve. Each calibration solution in the series shall meet the following requirements:
a. Without adding the test sample,
contains the test component in known and accurate amount;
can be determined by molecular absorption spectrum analysis method, and the measured absorbance value is the same as the absorbance value of the sample solution with the same concentration.
Note: The calibration solution with zero amount of the test component added is called zero calibration solution. Approved by the Ministry of Chemical Industry of the People's Republic of China on February 24, 1989 and implemented on December 1, 1989
3.B Test solution test solution
GB 1071389
The solution prepared by the test sample according to the molecular absorption spectrum analysis method. 8.7 Blank test solution blank test solution refers to a solution prepared in the same way as the test solution but without the test component. Blank test can be prepared by the following base samples: a. An equal amount of sample that has been processed to confirm that the content of the component to be tested is below the detection limit specified in the method, while other characteristics remain unchanged; b. An equal amount of substance that has the same or very similar components as the sample except that it does not contain the component to be tested; b. A substance that is inert under the test conditions and does not contain the component to be tested (such as water); d. No sample is added.
Based on the interference of the matrix on the component to be tested and its elimination, and the principle of consistency in the determination sensitivity of the component to be tested in the blank test solution and the test solution, one of the above four samples is selected. 3.8 Sample solutionsamplesolution
A solution prepared for direct absorbance measurement. It can be prepared by diluting a certain amount of the test solution according to the sensitivity of the instrument and the selected calibration curve range. 3.9 Reference solutionreference solution When measuring the absorbance of the sample solution or calibration solution, it is used as a comparative solvent or compensation solution. 3.10 Compensation solution compensationsolution is a solution prepared to eliminate the characteristic absorption of the reagent itself (sometimes to eliminate the absorption caused by the component to be measured in the sample, etc.). It is used when the solvent cannot be used as a reference solution. Compensation solutions include:
calibration compensation solution;
"zero" calibration compensation solution;
sample compensation solution:
d blank test compensation solution.
Note: The concentration of all reagents used in the preparation of these solutions should be the same as their concentration in the corresponding solution (calibration bath series. Zero calibration solution. Sample solution, blank test solution). 4 Basic requirements for the preparation of standards for molecular absorption spectral analysis methods 4.1 Basic requirements for the preparation of standards for molecular absorption spectral analysis methods should comply with the provisions of Articles 3.1 to 3.5 of GB1.1. 4.2 The procedures should be written in the order specified in Chapter 5 of this standard on the “Composition of the Standard for Molecular Absorption Spectroscopy Analysis Methods”. They may be omitted only when the given provisions are not applicable. 4.3 If the materials to be analyzed are hazardous, they should be stated in the “Applicable Application” section of the analytical method standard, and the precautionary measures should be written in bold. If the reagents used are hazardous, the precautionary measures should be written in bold in the “Reagents and Materials” section. If the analytical steps are hazardous, the precautionary measures should be written in bold in Chapter 7 of this standard. .7.1.
5 Composition of molecular absorption spectroscopy analysis method standards The general composition and writing order of molecular absorption spectroscopy analysis method standards are as follows: Cover and first
Overview
Standard name
(See Article 6.1)
(See Article 6.1)
(See Article 6.2)
(See Article 6.3)
Main text
Supplementary
GB 10713--89
Subject content and scope of application
Used standards
Terms, symbols, codes
Reagents and materials
Instruments and equipment
Analysis procedures
Safety measures
Preparation of test solution
Preparation of blank test solution (or blank test)Calibration
Preparation of calibration solution series
Generation of absorbing compounds of calibration solution
Calibration compensation solution
Absorbance measurement
Drawing of calibration curve
Generation of absorbing compounds of sample solution
Sample compensation solution
Absorbance measurement
Blank test
Presentation of analysis results
Precision
Additional notes
Not all of the above components need to be included in any standard. Add or reduce according to the specific situation of the object.
6 OverviewWww.bzxZ.net
(See Article 7.1)
(See Article 7.2)
(See Article 7.2)
(See Article 7.3)
(See Article 7.4)
(See Article 7.5)
(See Article 7.6)
(See Article 7.7)
(See Article 7.7.1)
(See Article 7.7.3)
(See Article 7.7.4)
(See Article 7.7.6)
(See Article 7.7.5. 1)
(see 7.7.5.2)
(see 7.7.5.3)
(see 7.7.5.4)
(see 7.7.5.5)
(see 7.7.6)
(see 7.7.6.1)
(see 7.7.6.2)
(see 7.7.6.3)
(see 7.7.6.4)
(see 7.8)
(see 7.9)
(see 7.10)
(See Chapter 8)
(See Chapter 1)
Which contents of a standard should be included? 6.1 The cover and front page of the absorption spectrum analysis method standard should comply with the provisions of Article 5.1 and Article 5.2 of GB131.1. 6.2 The name of the absorption spectrum analysis method standard should comply with the provisions of Article 5.3 of GB1.1, and should also clearly state the objects to which the analysis method can be applied, the components to be measured, and the characteristics of the analysis method. 6.3 The introduction of the molecular absorption spectrum analysis method standard should comply with the provisions of Article 5.4 of GB1.1. 7 Body
7.1 The title, content and scope of application of the molecular absorption spectrum analysis method standard The title, content and scope of application of the molecular absorption spectrum analysis method standard should comply with the provisions of Article 6.1 of GB1.1, and should generally clearly specify the objects to which the analysis method is applicable and the content range of the components to be measured. When interference exists, the interfering components and their limits should also be specified. 7.2 Reference standards and terms, symbols and codes for molecular absorption spectroscopy analysis methods3
GB 1071389
Reference standards and terms, symbols and codes for molecular absorption spectroscopy analysis methods should comply with the provisions of Article 6.2 and Article 6.3 of GB1.1, GR8322 and Chapter 3 of this standard. 7.3 Principle
The basic principles and main steps of the analysis method should be briefly described. If necessary, the main chemical equations should be listed and expressed as far as possible in terms of reaction formulas. Therefore, on the one hand, the physical and chemical principles of the analysis method in various preparatory stages before the determination (such as ashing, solution preparation, extraction, separation, complexation, etc.) should be described, and on the other hand, the characteristics of the method should also be described. Such as: a. Details and characteristics of the generation of light-absorbing compounds; b. Precautions during the generation or reaction of light-absorbing compounds; "c. The wavelength during measurement, and whether the wavelength meets the maximum absorption length of the spectrum. If not, the reason should be stated. 7.4 Reagents and materials
Should comply with the provisions of GB1.4 on reagents and materials, and should specifically state the preparation of standard solutions for the calibration solution series. The purity of the reagents should be specified. If necessary, the methods for purification and testing the purity of the reagents should be stated. 7.5: Instruments and equipment
Commonly used laboratory instruments do not need to be described, but the minimum requirements for the molecular absorption spectrometer to give a response must be specified, and the maximum allowable spectral bandwidth of the effective wavelength and the allowable fluctuation range of the nominal wavelength should be specifically indicated. If a special thickness of absorber is required The collection pool should be explained. If necessary, the inspection of the main performance of the molecular absorption spectrometer should also be explained. 7.6 Samples
Should comply with the provisions of "samples" in GB1.4, and explain all the steps for sample preparation. Note that when preparing samples, if there are special requirements, additional instructions must be given. 7.1 Analysis steps
The content described in this article is not applicable to all situations. Sometimes, in order to prepare one or several solutions specified in this article, certain preparatory tests (such as adjusting the pH value to meet the requirements of the measurement conditions) or control tests (for example, to adapt to certain special requirements of the solution medium, it is necessary to control the quality and dosage of the reagents, etc.). Therefore, in order to make the main text easy to understand and the methods easy to master, the standard writer may add the corresponding content to the article. Between the specified thin strips. When writing the standard, include all the contents specified in this article as much as possible and write them in the given order. 7.7.1 Safety measures
If there are dangers such as explosion, fire or poison in the analysis steps, they should be marked in bold and preventive measures should be indicated. If detailed safety measures or first aid methods are required, they can be written in the appendix (reference). 7.7.2 Test materials
This article should be in accordance with the provisions of GB1.4 on "test materials" and the amount of test materials used for the test should be stated (by mass or volume). 7.T.3 Preparation of test solution
Since the amount of test material is only an approximate amount for guidance, it can be appropriately increased or decreased with the sensitivity of the instrument and the selected calibration curve range. Therefore, the maximum and minimum allowable concentrations of the test solution and sample solution samples need to be based on the calibration curve The linear working range is determined. All chemical or physical treatments that must be performed on the sample for analysis before the absorbing compound develops color should be accurately described, and factors that may affect the analysis results should be explained. 7.7.4 Preparation of blank test solution (or blank test) The title of this clause depends on the content. If the content does not include the analytical steps for the generation of absorbing compounds, it is referred to as "Preparation of blank test solution", otherwise it is called "blank test".
There are also substantial differences in the above two cases. Sometimes the content should be described in detail, otherwise it will affect the measurement results. For example, due to the absence of certain components of the sample to be tested in the blank test solution, some conditions of the blank test solution and the sample solution (such as pH value) may not be completely the same. Therefore, the preparation method should be described in detail.
GB 10713-89
b. When the method for preparing the test solution is used to prepare the blank test solution, the content of this clause can be briefly mentioned in the "Preparation of the test solution" clause:
In some cases, the zero solution in the calibration solution series can replace the blank test solution. Ct
7.7.5 Calibration
7.7.5.1 Preparation of calibration solution series
This clause shall specify the volume of standard solution required to prepare a series of calibration solutions from zero to the maximum allowable amount of the component to be tested. The specified range of the calibration solution series is only an approximate guideline range. Since it varies with the sensitivity of the instrument, it can be increased or decreased appropriately. In order to obtain the best test conditions, the analyst should adjust the final dilution of the test solution. 7.7.5.2 Generation of calibration solutions for absorbent compounds This clause shall detail the preparation steps of each calibration solution in the calibration solution series used for absorbance measurement. If necessary, it shall state:
a. Precautions in the process of generating the absorbent compound and the order of adding various reagents, time intervals and time required to obtain the generation of the absorbent compound. If there is no stipulation, it is stated that the generation reaction of the absorbent compound is complete and instantaneous; b. The temperature at which the generation reaction of the absorbent compound is completed: the stability time of the absorbent compound.
If there are no such provisions, it means:-All operations can be carried out continuously!
b. It can be operated between 10 and 40℃,
c. The absorbance of the absorbing compound does not need to be calibrated over time. 7.7.5.3 Calibration compensation bath
If a solution is to be prepared to compensate for the calibration solution series, the entire preparation process (or only the correction process of the calibration solution series) should be stated.
7.7.5.4 Absorbance measurement
This clause should state the following details:
7.7.5.4.1 The measurement wavelength should be stated. Usually, an absorption spectrum should be drawn to find the maximum absorption wavelength of the spectrum related to the instrument used, but sometimes in order to avoid interference from other absorbing substances, a wavelength at a non-value can also be selected for some special analyses. 7.7.5.4.2 The reference solution for adjusting the instrument to zero absorbance should be stated. This reference solution can be! It is best to use water or solvent used in the method.
b. Calibration compensation solution;
c. Blank test solution;
d. Calibration solution series: i. Zero calibration solution. No matter which of the above solutions is used, it will have little effect on the measured properties (such as sample characteristics, properties of absorbing compounds and characteristics of analytical steps, etc.).
When a special reference solution must be used, it should be stated and emphasized with the word "must". 7.7.6.4. 3 The measurement temperature should be stated
If this clause does not make specific provisions on the temperature, it means that it can be operated between 10 and 40 degrees Celsius without any special measures. However, it is only required that the volume change caused by the temperature fluctuation of the solution to be tested (including various reference solutions) must be small enough to be ignored. Note: For single beam absorption spectrometers, when using different temperatures between 1°C and 44°C, the operating temperature must be calibrated according to the requirements of the instrument.
7.7.5.4.4 The thickness of the absorption cell applicable to the calibration solution series should be stated. 7.7.5.5 Drawing of calibration curve
Plot the measured absorbance values against the concentrations of the calibration solution series or determine a linear regression equation, and state the linear range of the curve or equation.
The following points should be noted when drawing the calibration curve: GB10713-89
Generally, there should be at least five points (excluding the zero point), specify the conditions for redrawing or specify that the absorbance of the calibration curve should be measured at the same time as each sample measurement. 7.7.6 Determination
7.7.6.1 Generation of absorbent compounds in sample solution This item should state the operating steps for preparing the sample solution, and the other contents are the same as 7.7.5.2. 7.7.6.2 Sample compensation solution
This item can be written with reference to 7.7.5.3.
7.7.6.3 Absorbance measurement
The content of this item is the same as 7.7.5.4. The contents of "Absorbance Measurement" for completing the calibration solution series are equivalent. The reference solution used to adjust the instrument absorbance to zero can be: water or solvent used in the method, sample compensation solution, blank test solution; zero calibration solution in the calibration solution series. d. When these solutions are equivalent, it is best to use the water or solvent used in the method as the reference solution, and add a note stating "If the obtained solution is only used to correct the results, other reference solutions can be used equivalently". In addition, when a special reference solution must be used, it should be stated and emphasized with the word "must".
7.7.6.4 Blank test
If the content of 7.7.4 is limited to the preparation of blank test solution, this content should be written. 7.8 Expression of analysis results
This clause shall give the calculation formula and state how to calculate the desired characteristic value from the following values: the calibration curve obtained according to 7.7.5.5,
the measurement results obtained according to 7.7.6.3,
the measurement results obtained according to 7.7.6.4, if necessary, d.
the amount of sample used to prepare the test solution (see 7.7.2) the dilution multiple between the test solution and the sample solution. In addition, the meter display unit used shall be clearly stated. 7.9 Precision
The precision (i.e. repeatability and reproducibility) of the analytical method shall generally be stated, and the requirements and writing of precision shall be in accordance with the provisions of the relevant precision standards.
7.10 Others
In addition to the above nine technical contents, other contents may be added according to the characteristics and needs of the molecular absorption spectrum analysis method, such as explanations of special circumstances, test reports, relevant charts, etc. 8 Supplementary part
Reasonable preparation of other technical
The appendix and additional instructions of the absorption spectrum analysis method standard shall comply with the provisions of Chapter 7 of GB1.1. Additional instructions:
This standard was issued by the Standardization Research Institute of the Ministry of Chemical Industry. This standard is undertaken by the Standardization Research Institute of the Ministry of Chemical Industry. The main drafter of the draft standard is Zhang Fang.
Chinese People's Republic of China
National Standard
Molecular Absorption Spectral Analysis Method Standard
Compilation Regulations
GB 10713 89
Published by China Standards Press
(Erlihe, Fuwai, Beijing)
Printed by Beijing Printing Factory of China Standards Press Distributed by Xinhua Bookstore, Beijing Distribution Office Sold by Xinhua Bookstores in various places Copyright is exclusive and reproduction is prohibited
Format 880×1230 1/16 Printing Sheet 3/4 Number of Words 12 00 First Edition December 1989
First Printing December 1989
Print 1 3 00℃
Book number: 155066·1-6776
Price: 0.75 yuan
Standard date: 128-34
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