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JJF 1574-2016: Program of Pattern Evaluation of Atomic Absorption Spectrophotometers
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Program of Pattern Evaluation of Atomic Absorption Spectrophotometers
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JJF 1574-2016
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Basic data | Standard ID | JJF 1574-2016 (JJF1574-2016) | | Description (Translated English) | Program of Pattern Evaluation of Atomic Absorption Spectrophotometers | | Sector / Industry | Metrology & Measurement Industry Standard | | Classification of Chinese Standard | A61 | | Word Count Estimation | 33,324 | | Date of Issue | 2016-06-27 | | Date of Implementation | 2016-09-27 | | Regulation (derived from) | State Administration of Quality Supervision, No.66 of 2016 | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine | JJF 1574-2016: Program of Pattern Evaluation of Atomic Absorption Spectrophotometers---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.
Program of Pattern Evaluation of Atomic Absorption Spectrophotometers
National Metrological Technical Code of the People's Republic of China
Atomic Absorption Spectrometer Type Evaluation Outline
2016-06-27 released
2016-09-27 implementation
State Administration of Quality Supervision, Inspection and Quarantine issued
Atomic Absorption Spectrophotometer
Type evaluation outline
Responsible unit. National Physical and Chemical Metrology Technical Committee
The main drafting unit. China Institute of Metrology
Participated in the drafting unit. Xinjiang Uygur Autonomous Region Measurement and Testing Research Institute
This specification entrusts the National Physical Chemistry Metrology Technical Committee to explain
The main drafters of this specification.
Cui Yanjie (China Institute of Metrology)
Wu Bing (China Institute of Metrology)
Participate in the drafters.
Bai Xu (Xinjiang Uygur Autonomous Region Measurement and Testing Institute)
table of Contents
Introduction (Ⅲ)
1 Scope (1)
2 References (1)
3 Overview (1)
4 legal management requirements (2)
4.1 Unit of measurement (2)
4.2 Metrological markings and metrological instruments (2)
5 Metering requirements (2)
6 General technical requirements (3)
6.1 Appearance (3)
6.2 Power Environment Adaptability (3)
6.3 Adaptation of climate and environment (3)
6.4 Stability (3)
7 type evaluation item (3)
8 Technical data and test samples to be submitted by the applicant unit (4)
8.1 Technical Information (4)
8.2 Number of prototypes provided (4)
8.3 Use of prototype (4)
9 Test methods and conditions for type evaluation items (4)
9.1 Preparation before trial (4)
9.2 Appearance (4)
9.3 wavelength indication error and repeatability test (4)
9.4 Spectral Bandwidth Deviation (5)
9.5 Baseline stability (6)
9.6 Edge Energy (6)
9.7 detection limit (7)
9.8 Measurement Repeatability (8)
9.9 Linearity error (9)
9.10 Apparent atomization rate (10)
9.11 Background correction capability (10)
9.12 Power environment adaptability test (11)
9.13 Climate Environment Adaptability Test (12)
9.14 Stability (13)
9.15 Judgment of type evaluation result (13)
10 Measuring instruments and equipment for use in test items (13)
Appendix A Atomic Absorption Spectrophotometer Type Evaluation Original Recording Format (15)
Introduction
This specification is based on JJF 1015-2014 "General specification for evaluation of measuring instruments", JJF 1016-2014
Preparation of the outline of the outline of the evaluation of the outline of the instrument.
The technical indicators of this specification refer to JJG694-2009 "atomic absorption spectrophotometer", GB/T 11606-
2007 "Analytical Instruments Environmental Test Method", GB/T 21187-2007 "Atomic Absorption Spectrophotometer" and other technical literature
, Which is the primary reference standard, the standard is for reference only.
This specification is the first release.
Atomic Absorption Spectrometer Type Evaluation Outline
1 Scope
This specification is applicable to the type evaluation of the atomic absorption spectrophotometer classified as 46121500.
2 reference file
This specification refers to the following documents.
Atomic Absorption Spectrophotometer JJG694-2009
Environmental testing methods for analytical instruments GB/T 11606-2007
Atomic Absorption Spectrophotometer GB/T
For dated references, only the dated edition applies to this specification; references that are not dated
, The latest version (including all modifications) applies to this specification.
3 Overview
Atomic absorption spectrophotometer is the use of flame or graphite furnace temperature of the sample to be measured in the atomic element, ground
Atomic absorption of the characteristics of the wavelength of radiation, according to different elements to absorb different wavelengths, different concentrations of different absorption to carry out
Quantitative and qualitative analysis of each element. The main structure of the instrument, including light source, atomizer, monochromator, detection system four
Part, in which the atomizer can be divided into two kinds of flame and graphite furnace. The measurement principle is based on the Langbobier light absorption
law.
Abs = -lg
I0 = -
lgT = kcL (1)
Where.
Abs - absorbance;
I - transmitted light intensity, cd;
I0 --- incident light intensity, cd;
T --- transmittance;
k - absorption coefficient;
c - the concentration of the element under test in the sample;
L - light through the atomic path of the instrument, cm.
The main structure of the instrument block diagram shown in Figure 1.
Figure 1 instrument structure diagram
The instrument can be divided into single beam type and double beam type; according to the type of atomizer can be divided into flame atomization
And no flame (graphite furnace) atomizer.
4 legal management requirements
4.1 Unit of measurement
Atomic absorption spectrophotometer should be used in the legal unit of measurement.
4.2 Measurement of legal signs and measuring instruments
Atomic absorption spectrophotometer must be in the instrument nameplate or panel, header and other obvious parts marked the legal system mark
And the marking of the measuring instrument, its mark, number and description must be legible, solid and reliable.
4.2.1 Metrological legal symbols generally include the following.
4.2.1.1 Manufacture of measuring instruments License mark and number (test prototype can be left with the corresponding position, only the domestic instrument
Device).
4.2.1.2 Instrument type approval mark and number (this item is non-mandatory, the test prototype can leave the corresponding bit
Set).
4.2.2 Metrological instruments generally include the following.
Instrument name, manufacturer name, specification (model), date of manufacture, factory number. Have special requirements for installation
Atomic absorption spectrophotometer, there should be instructions for installation instructions.
5 metering requirements
Atomic absorption spectrophotometer metering performance requirements in Table 1.
Table 1 Metrological performance indicators
project
Measurement performance
Flame Atomizer Graphite Furnace Atomizer
5.1
Wavelength indication error
Difference and repeatability
The wavelength indication error does not exceed ± 0.5nm,
Wavelength repeatability is not greater than 0.3 nm
The wavelength indication error does not exceed ± 0.5nm,
Wavelength repeatability is not greater than 0.3 nm
5.2 spectral bandwidth deviation of not more than ± 0.02nm does not exceed ± 0.02nm
5.3 Baseline stability
Zero drift absorbance does not exceed ± 0.005/30min;
Instantaneous noise absorbance ≦ 0.005
5.4 Edge energy
Spectral line background value/spectral peak should be ≤ 2%
Instantaneous noise absorbance should be ≤ 0.02
Spectral line background value/spectral peak should be ≤ 2%
Instantaneous noise absorbance should be ≤ 0.02
5.5 detection limit ≤ 0.01μg · mL-1 ≤ 1pg
5.6 Measurement repeatability ≤ 1.0% ≤4.0%
5.7 Linearity error not exceeding ± 10% No more than ± 15%
5.8 Apparent atomization rate ≥8% -
5.9 background correction capacity ≥ 30 times ≥ 30 times
Note.
1. For wavelength automatic calibration of the instrument does not carry out wavelength indication error and repeatability measurement;
2. Manual Wavelength Spectral Bandwidth Measurements were measured with resolution measurements instead of Mn279.5 nm and 279.8 nm line sweep
Description, the peak and valley energy should not exceed 40%.
General technical requirements
6.1 Appearance
The adjustment buttons, buttons and switches can work properly, no loosening phenomenon.
6.2 Power environment adaptability
When the supply voltage changes at 220V ± 22V, the measurement shall be made to meet the requirements.
6.3 Climate and environmental adaptability
6.3.1 high temperature environment experiment. the instrument is in normal working condition, placed in the ambient temperature of 35 ℃ ± 2 ℃ test
Box, the continuous test time of 2h, the instrument should be able to work properly, the 5.6 measurements, should meet the requirements.
6.3.2 low temperature environmental test. the instrument is in normal working condition, placed in the ambient temperature of 10 ℃ ± 2 ℃ test
Box, the continuous test time of 2h, the instrument should be able to work properly, the 5.6 measurements, should meet the requirements.
6.4 Stability
After the operation of 4h after the measurement repeatability indicators should meet the requirements of Table 1, paragraph 5.6.
7 type evaluation item
The list of type evaluation items is shown in Table 2.
Table 2 List of types of evaluation items
Type Evaluation Item Type Requirement
Legal tube
Claims
Unit of observation 4.1
Measurement of legal signs and measuring instruments Identifying items 4.2
Metering
Claim
Wavelength Indication Error and Repetitive Test Item 5.1
Spectral Bandwidth Deviation Test Item 5.2
Baseline stability test item 5.3
Edge Energy Test Item 5.4
Detection limit test item 5.5
Measure repeatability test item
Linear error test item 5.7
Apparent atomization rate test item 5.8
Background correction capability test item 5.9
General
technology
Claim
Appearance observation item 6.1
Power environment adaptability test item 6.2
Climate and Environment Adaptability Test Item 6.3
Stability test items 6.4
8 Applicants should submit technical information and test prototype
8.1 Technical Information
The following technical information application units should be provided in duplicate.
It is accepted by the government metrological administrative department and entrusted with type evaluation
book";
---Product Standards;
--- assembly drawings, circuit diagrams and key parts list;
---user's Guide;
A test report made by a manufacturing unit or a technical organization.
8.2 The number of prototypes provided
8.2.1 For a single product, provide a prototype.
8.2.2 series of products
For a range of products, at least one third of each series of products with representative specifications of the product, each specification
The product should provide a prototype.
8.3 Use of the prototype
The prototype provided should be evaluated for all items.
9 Type of test items and test conditions
9.1 Preparation before trial
The instrument should be placed on the table smoothly, no direct light on the instrument, no strong magnetic field around, electric field interference;
No vibration; no strong airflow.
9.2 Appearance
9.2.1 Purpose of the test
Check whether the appearance of the instrument meets the requirements of 6.1
9.2.2 Test conditions
The ambient temperature is (20 ± 5) ℃, the relative humidity is not more than 85%, the AC supply voltage is (220 ± 22) V,
The AC supply frequency is (50 ± 0.5) Hz.
9.2.3 Test procedures
The instrument placed under the test conditions, so that it reaches the temperature and humidity balance, check the appearance and structure of the instrument
The requirements of 6.1.
Qualified Criteria
The results meet the requirements of 6.1 for the qualified, otherwise failed.
9.3 Wavelength indication error and repeatability test
9.3.1 Purpose of the test
Check whether the wavelength indication error and repeatability of the atomic absorption spectrophotometer meet the requirements of 5.1.
Note. This measurement is not performed for instruments with wavelength auto-calibration.
9.3.2 Test conditions
With the requirements of 9.2.2.
9.3.3 Test equipment
Performance Tested Atomic Absorption Mercury Hollow Cathode Lamps.
9.3.4 Test procedures
According to the provisions of the hollow cathode lamp operating current light mercury lamp, to be stable, the spectral bandwidth of 0.2nm conditions
, From the following mercury, neon lines 253.7 nm, 365.0 nm, 435.8 nm, 546.1 nm, 640.2 nm,
724.5nm and 871.6nm in accordance with the principle of uniform distribution, select three to five one by one to do three one-way (from short to long
Wave direction) to give the maximum energy of the wavelength indication as a measured value.
9.3.5 Data processing
And then calculated according to formula (2) and formula (3).
Wavelength indication error Δλ = 1/3 (ΣΔλ) (2)
Where.
Δλ --- The instrument automatically calibrates the given deviation, nm.
Wavelength Repeatability δλ = Δλmax - Δλmin (3)
Where.
Δλmax --- the maximum value of the third-order indication error of a line, nm;
Δλmin --- the minimum value of the third-order indication error of a line, nm.
9.3.6 Qualification Criteria
Atomic Absorption Spectrophotometer Wavelength Indication Error and Repetitive Results Meet the requirements of 5.1 for qualified, otherwise
qualified.
9.4 spectral bandwidth deviation
9.4.1 Purpose of the test
Verify that the spectral bandwidth deviation of the atomic absorption spectrophotometer meets the requirements of 5.2.
9.4.2 Test conditions
With the requirements of 9.2.2.
9.4.3 Test equipment
For the automatic scanning of the instrument using the test of atomic absorption of copper hollow cathode lamp; on the manual dial wheel instrument
Use the tested atomic absorption of manganese hollow cathode lamp.
9.4.4 Test procedures
Bright copper lamp, to be stable, the spectral bandwidth of 0.2nm conditions, the 324.7nm line scan,
The half width of the scanning line is then measured. Measurements are shown in Figure 2.
Figure 2 half-width measurement icon
Note. For instruments with variable wavelengths, this is replaced by resolution measurements due to the minimum grading of wavelengths. The method is as follows. point
Bright manganese lamp, to be stable, the spectral bandwidth of 0.2nm, adjust the photomultiplier tube high pressure, so that the energy of 279.5nm line
To 100, and then scan the measurement of manganese double line, this time should be able to clearly distinguish between 279.5nm and 279.8nm two lines, and
The energy between the two lines should not exceed 40%.
9.4.5 Data processing
Spectral bandwidth deviation = (λ2 - λ1) -0.2nm.
9.4.6 Qualification Criteria
Atomic absorption spectrophotometer spectral bandwidth deviation in line with the requirements of 5.2 qualified, otherwise failed.
9.5 Baseline stability
9.5.1 Purpose of the test
Verify that the baseline stability of the atomic absorption spectrophotometer meets the requirements of 5.3.
9.5.2 Test conditions
With the requirements of 9.2.2.
9.5.3 Test equipment
The use of tested atomic absorption of copper hollow cathode lamp.
9.5.4 Test procedures
In the 0.2nm spectral bandwidth conditions, according to the best flame conditions of copper, ignited acetylene/air flame, suction
Secondary distilled water or deionized water, after 10min, with "instantaneous" measurement, or time constant is not greater than 0.5s,
Wavelength of 324.7nm, for measurement.
9.5.5 Data processing
Record zero drift in 30 min (based on starting point) and instantaneous noise (peak-to-peak).
9.5.6 Qualification Criteria
Atomic Absorption Spectrophotometer measures baseline stability in accordance with 5.3 requirements for compliance, otherwise unqualified.
9.6 Edge energy
9.6.1 Purpose of the test
Verify that the edge energy of the atomic absorption spectrophotometer meets the requirements of 5.4.
9.6.2 Test conditions
With the requirements of 9.2.2.
9.6.3 Test equipment
Respectively, using the test of atomic absorption of arsenic, cesium hollow cathode lamp.
9.6.4 Test procedures
Lit arsenic and cesium lamp, to be stable, according to the instrument recommended the best working conditions set spectral parameters, response time
Not more than 1.5s under the conditions of arsenic 193.7nm and cesium 852.1nm lines were 9.6.4.1 and 9.6.4.2
measuring.
9.6.4.1 Measure the background value/peak at the peak energy of the two spectral lines to be optimized.
9.6.4.2 Measure the instantaneous noise of the line, the maximum instantaneous noise (peak-to-peak) in 5 min.
9.6.5 Qualification Criteria
The atomic energy of the atomic absorption spectrophotometer conforms to the requirements of 5.4, otherwise it is unqualified.
9.7 detection limit
9.7.1 Purpose of the test
Check whether the detection limit of atomic absorption spectrophotometer meets the requirements of 5.5.
9.7.2 Test conditions
With the requirements of 9.2.2.
9.7.3 Test equipment
Flame Atomizer. Tested Atomic Absorption with Copper Hollow Cathode Lamp; Graphite Furnace Atomizer. Tested Original
Sub-absorption with cadmium hollow cathode lamp; atomic absorption test with copper, cadmium solution standard material, copper uncertainty is better than equal
1% (k = 2); cadmium uncertainty is better than 2% (k = 2).
9.7.4 Test procedure
9.7.4.1 Flame atomization method for the detection of copper limits
The instrument parameters to the normal working state, with blank solution zero, according to the instrument sensitivity conditions, select the system
Column 1. (0.0,0.5,1.0,3.0) μg · mL-1 or Series 2. (0.0,1.0,3.0,5.0) μg · mL-1
Copper standard solution, for each concentration point were repeated three times the determination of absorbance, take the average of three measurements, press
Linear regression method to find the slope of the working curve b. At the same time on the blank solution for 11 times the absorbance measurement, according to the public
Equation (4) calculates the blank standard deviation.
sA =
i = 1
(I0i-I0) 2
n-1
(4)
Where.
sA --- 11 standard deviation of blank measurement;
I0i --- absorbance of a single measurement;
I0 --- absorbance measurement average;
n - number of measurements.
Determination of Determination of Cadmium by Graphite Furnace Atomization Method 9.7.4.2
The parameters of the instrument transferred to the normal working condition, according to the instrument sensitivity conditions, select Series 1. (0.0,0.5,
1.0, 3.0) ng · mL-1 or series 2. (0.0,1.0,3.0,5.0) ng · mL-1 cadmium standard solution,
A concentration point were repeated three times the determination of absorbance, take the average of three measurements, according to the linear regression method to find workers
As the slope of the curve b, according to formula (5) to calculate the sensitivity of the instrument measured S. While the blank solution for 11 times the light absorption
Degree of determination, according to formula (4) to calculate.
S = b/V (5)
Where.
S --- sensitivity, pg-1;
b - slope of the working curve absorbance, (ng · mL-1) -1;
V --- sampling volume, μL.
9.7.5 Data Processing
9.7.5.1 Calculate the detection limit of copper by flame atomization method according to formula (6).
CL = 3sA/b (6)
Where.
CL --- detection limit, μg · mL-1;
sA --- calculation method see formula (4);
b - linear fit slope, (μg · mL-1) -1.
9.7.5.2 Calculate the detection limit of cadmium by graphite furnace atomization method according to formula (7).
QL = 3sA/S (7)
Where.
QL --- detection limit, pg;
sA --- calculation method see formula (4);
S --- calculation method see formula (5).
Qualified Criteria
Atomic absorption spectrophotometer detection limit in line with the requirements of 5.5 qualified, otherwise failed.
9.8 Measure repeatability
9.8.1 Purpose of the test
Check whether the repeatability of the atomic absorption spectrophotometer meets the requirements of 5.6.
9.8.2 Test conditions
With the requirements of 9.2.2.
9.8.3 Test equipment
With 9.7.3.
9.8.4 Test procedure
9.8.4.1 Flame atomization method for measuring copper repeatability
In the determination of 9.7.4.1, select a series of standard solution in a concentration of solution, the absorbance in the
(RSD), see formula (8), and the relative standard deviation (RSD) is obtained in the range of 0.1 to 0.3,
That is, the instrument to measure the repeatability of copper.
9.8.4.2 Determination of cadmium repeatability by graphite furnace atomization
In the determination of Article 9.7.4.2, select a series of standard solution of a concentration of solution, the absorbance in the
(RSD), see formula (8), and the relative standard deviation (RSD) is determined in the range of 0.1 to 0.3,
That is, the instrument measured cadmium repeatability.
9.8.5 Data processing
Repetitive calculation is as follows.
RSD =
i = 1
(Ii-I) 2
n-1 ×
100% (8)
Where.
RSD --- relative standard deviation,%;
Ii --- absorbance of a single measurement;
I - absorbance measurement average;
n - number of measurements.
9.8.6 Qualification criteria
Atomic Absorption Spectrometer Repeatability Complies with 5.6 requirements for qualified, otherwise unqualified.
9.9 Linearity error
9.9.1 Purpose of the test
Check whether the linear error of the atomic absorption spectrophotometer meets the requirements of 5.7.
9.9.2 Test conditions
With the requirements of 9.2.2.
9.9.3 Test equipment
With 9.7.3.
9.9.4 Test procedure
9.9.4.1 Linear error of copper by flame atomization
Measured with 9.7.4.1.
9.9.4.2 Determination of Cadmium Linearity by Graphite Furnace Atomization
Measured with 9.7.4.2.
9.9.5 Data processing
After the operation of 9.8.4.1 and 9.8.4.2 is completed, the standard curve measurement is calculated according to the formulas (9) to (11)
Intermediate point (Series 1 Calculate Cu. 1.0 μg · mL-1/Cd. 1.0 ng · mL-1; Series 2 Calculations
Cu. 3.0 μg · mL-1/Cd. 3.0 ng · mL-1) Δxi.
Linear equation. Ii = a bci (9)
ci =
Ii-a
(10)
Linear error. Δxi =
ci-csi
csi x
100% (11)
Where.
Ii --- the average of the three absorbance measurements;
ci - the measured value of the measured value, calculated by the linear equation, μg · mL-1 or ng · mL-1;
csi - the standard concentration of the standard solution at point i, μg · mL-1 or ng · mL-1;
a - the intercept of the working curve;
b - slope of the working curve, (μg · mL-1) -1 or (ng · mL-1) -1.
9.9.6 Qualification Criteria
Atomic absorption spectrophotometer linear error in line with the requirements of 5.7 qualified, otherwise unqualifi...
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