Some standard content:
National Metrology Verification Regulations of the People's Republic of China JJG 964—2001
Capillary Electroptoresis Instrument
Capillary Electroptoresis Instrument2001-07-06 Issued
2001-10-01 Sold and implemented
The General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China issued JJG 964—3001
Verification Regulations of Capillary Electrophoresis Instrument
YcriricatinnRcgulationof
Capillary Electrophoresis InstrumentJJG 964—2001
This regulation was approved by the State Administration of Supervision, Inspection and Quarantine on October 6, 2001, and implemented on October 1, 2001
Responsible unit: National Physical and Chemical Metrology Technical Committee Main drafting unit:
: Beijing Basic Measurement and Testing Institute
Participating drafting unit:
Chaojian Provincial Product Science and Technology Institute
Baoding Commercial New District People's Benefit Business Science Institute Beijing New Technology Application Institute
This regulation is entrusted to the National Physical and Chemical Metrology Technical Committee for interpretation. Main drafters of this regulation:
Liu Zengming
Zheng Kepeng
Participating drafters:
7 Tianhui||tt ||Shi Yafen
J.964-2001
(Hebei Testing Institute)
(Beijing Institute of Material Science and Engineering)
(Hebei Institute of Metrology and Testing)
(Fujian Institute of Science and Technology) (Baoding High-tech Zone Tianhui Separation Science Institute) (Beijing Institute of New Technology Application)
Scope·
Overview·
Performance requirements of measurement
General technical requirements
Control of measuring instruments·
Appendix A Preparation of standard solution
Appendix B
Format of verification certificate (back)
Appendix ℃
Format of verification record
JJG J64—2001
1Fundamentals of Industry
J.:904--2001
Procedure for verification of capillary electrophoresis
This specification describes the determination, subsequent verification and in-service inspection of positive capillary electrophoresis instrument with ultraviolet detector.
2 Overview
The capillary electrophoresis instrument (hereinafter referred to as the instrument) is a kind of instrument for the purpose of separation and separation of charged particles in a medium solution at different speeds under the action of a high voltage electric field. The detection is carried out based on the activity time and response value of each component, and the qualitative and quantitative analysis is carried out based on the activity time and response value of each component. The support of the capillary electrophoresis is an elastic quartz capillary. The instrument mainly consists of a high positive frequency, a sample injector, a capillary column, a detection system, a data processing system and other parts. The working principle is shown in Figure 1.
Working principle of medical equipment
3. Measurement performance requirements
Heat treatment system
Medium installation length: -2m; filter semi-amplitude: 15t (constant wavelength UV measurement) 3.2 Wavelength indication error: -2m; length repeatability: 1m continuous adjustment length UV measurement density, .3.3
Line source shift: 0.02A0hs
Baseline noise: 0.0005 AU.
Limit: 1×10l (copper element B
Medium source
JJG 964—2001
3.6.1 Voltage range: [--30V, indication error is ±2.0%3.6.2 Current range: --300xA, indication error is ±3.0%, 3.6.3 Stability
3mm electric field error 1.5%
3.7 Qualitative and quantitative measurement repeatability
3.7.1 Qualitative measurement repeatability error (8 measurements) 1.5%. 3, .2 Qualitative measurement repeatability error [8 measurements 3, heart%4 General technical requirements
4.1 Appearance of the instrument
4.1.1 The instrument should have the following signs: name, model, manufacturer name, production date, product number, logo, power supply voltage and frequency, maximum power, 4.1, 2 The instrument should be stable. On the workbench, all the accumulated hardware should be tightened well, and all adjustments should be made. Regulators, buttons and switches can work normally
4.1.3 The cable connectors should be tightly matched and in good contact. 4.2 Gas system: Under normal working conditions, block the end of the gas circuit and connect the joints with membrane liquid. There should be no gas pool.
4.3 Insulation resistance: The insulation resistance should be greater than 1M.5 Measuring instrument control
Measuring instrument control includes: initial calibration, post-calibration and inspection during use. 5.1 Calibration conditions
S.1.1 Calibration environmental conditions
5.1.1.1 Ambient temperature: (20=5)
5.1.1.2 Ambient humidity: Relative temperature 85%R} Power supply: (22022)V, (5±5)Hz5.1.2
5.1.3 Calibration equipment
Stopwatch: Graduation value 0.1 s
Analytical balance, maximum weighing 200: minimum scale, 1mg Current: -50A, 1. level
Electrostatic voltage meter: 0--30kV, 0.5 level
Insulation resistance meter: 5V, ~5M, 1.1 level: Resistance: 22M0, 1.0 level
5.1.4 Standard push substances and reagents
5.1.4.1 Secondary reagents/% (analytical pure)
5.1.4.2 Sodium hydrogen phosphate ( Analytical purity). 5.1.4.3 UV absorption standard liquid GEW (E) 130066: 2
5.2 Verification items and verification methods
5.2.1 Appearance inspection
JJG964—2001
Perform appearance and preliminary inspection according to 4.1-1.2.5.2.2 Verification of commercial voltage power supply
5.3.2.1 Verification of voltage indication error
Connect the electrostatic meter to a high voltage The output voltage of the power source is measured by evenly selecting 6 points (including the maximum nominal output voltage) within the range of the whole program, measuring the output voltage of the display point, calculating the indication error of each point according to formula (1), and taking the maximum value as the voltage indication error.
V#, V×100%
Where: Vindicator——voltage indication error, (%): Vmeasured voltage value at each point, kV
Vstandard——nominal voltage value at each point, kV=
5.2.2.2 Current indication
Connect the 22V battery and the battery meter to the output end of the high-voltage power supply, adjust the instrument to the maximum rated output current, and read the minimum value of the current display: Calculate the output current indication error according to formula (2): [h]
× 100%
Where: Display: voltage drop indication error, (mA - measured current value, mA):
I: instrument maximum rated output current value, eA5.2.2.3 Power supply setting
After the instrument is preheated for 30 min: Set the output pressure of the box to 20 kV, connect the electrostatic voltmeter to the high voltage output terminal of the power supply, observe continuously for 3min, record the maximum and minimum values recorded by the voltmeter, the ratio of the difference between the maximum and minimum values to the set output voltage value is the ideal value of the power supply, S.2.3 Verification of UV detector performance
5.2.3.1 Verification of wavelength indication error and repeatability 5.2.3.1.1: Verification of the center wavelength and half width of the detector outside the fixed wavelength band Take out the filter equipped with the detector, and verify the center wavelength (peak wavelength) and half width according to 11812-1993 "Verification Procedure for Filters" , its error and flat width should meet the requirements of series 1. 5.2.3.1.2 The minimum value error and single pump performance of the continuously adjustable wavelength ultraviolet detector are calibrated using external absorption standard solution at 235, 257, 313nm and 350nn:4 points to calibrate the wavelength indication error
. Set the detector wavelength at 5 points lower than the calibration wavelength (for example, when calibrating 257, the detector wavelength is first adjusted to 252m), and change the wavelength with time 】m to obtain the wavelength characteristic curve. The wavelength corresponding to the peak and trough of the curve is the measurement wavelength of that point. Repeat the measurement 3 times and take the average. The difference between the average value of the measured wavelength and the standard wavelength is the difference. Use the same centrifugal method to calibrate the other 3 points. The difference between its length and the minimum value is the wavelength. 5.2.4 Static step-by-step inspection and calibration should be carried out according to the following conditions: 251: The back of the hair is empty, the machine is turned on for 30 days, and the value of 1 is calculated. 5.2.5 Detection limit
Under the condition of the receiver, the wavelength of the multi-device is adjusted to 2541, using 75×40 physical capillary relay, temperature 25, medium pressure 15kV, this foreign pressure SP violation sample time H3: (gas positive): height difference 20c, time 180: (position ~ let the pole line play after, use 20:1 hydrogen phosphate as the flushing rate liquid, the concentration of the liquid should be 21U-:g/m3, reverse reading the sample 3 times, the potential average of the single peak height:
The detection limit is defined as twice the base The line case represents the highest concentration of the substance, and the detection limit is calculated by formula (3).
2H, /
formula "initial detection limit (minimum annual concentration of the substance, H-sound quotient, mm:
-sample concentration, m:
I-substance peak height, nm-
5.2.6 Qualitative and quantitative measurement to determine the reproducibility (3)
Press the proposed route together, stop the card at the normal working state: connect the remaining parts of 5.2.5, and obtain an injection area of 1×-/m Vitamin, drop, record the migration time and peak panel (peak): violation of the continuous year, connect formula (4: calculate the relative standard deviation quantitative
(100%
formula ten:
qualitative (fixed virtual) repeatability:
the first measurement of the Jiang migration time constant or the connection area end height: : - the mathematical average of the results of the measurement: measurement base number:
measurement base number:
5.2.7 Insulation resistance inspection
the power supply head is not connected to the power grid: use an insulation meter at the power supply line 5.2.3 Only the first device to be tested shall be fully tested according to the requirements of this test system. The company shall not conduct any subsequent test. 5.3 The final result of the test shall be issued if the test result is found to be in compliance with the requirements. If the test result is not in compliance with the requirements, a final certificate shall be issued, and the unqualified items shall be noted. 5.4 Test cycle 964—2001
The calibration cycle of capillary electrophoresis instrument shall not exceed 2 years. 5
Appendix A
A.1 Reagents
Reagent name
Vitamin B,
Disodium phosphate
Instruments and glass measuring vessels
Analytical balance
Base bottle
Soft-base bottle
JJG964—2www.bzxz.net
Preparation of standard solution
Formula
C,H:O,N-HCl
Na,HPO4-12H2
200g, graduation 0.1mE
[[],250 mil
A.32.0× 10-6 g/ml Vitamin B. Solution preparation name
Non-divided suction back
Non-divided suction arm
. Distilled water
Analytical pure
Analytical pure
Format/ml
On an analytical balance, accurately weigh 10.5 ml of vitamin B, solidify, and add 50 1. Prepare 420mmol/l of disodium hydrogen phosphate buffer solution. Weigh 1.79g of solid disodium hydrogen phosphate on an analytical balance, put it into a 50ml beaker, dilute it with distilled water, and transfer it to a 250m2/1 volumetric flask. Rinse the beaker 3 times with a small amount of sugar water. Wash the wave and put it into the volumetric flask, then dilute it with distilled water for a while, then pour it into the bottle for later use. 6
Appendix B
Gas system
Voltage indication error
Current indication error
Stability
Center wavelength error
Filter half width
Wavelength indication error
Wavelength stability
Baseline drift
Baseline noise
Detection limit
Qualitative measurement repeatability
Qualitative measurement complexity
Insulation resistance
Remarks:
IJG 964—2001
Verification certificate (back) format
Appendix C
Inspected unit
Only instrument model
Manufacture!
Appearance inspection
Gaoyu power supply
Electric current range and indication error
Electric current indication
Output medium voltage V
Indication error/(%)
2.2Current indication error
Maximum range of battery A
Amperemeter value A
Power supply stability
Power supply stability
Wavelength indication error and repeatability
JJC964—2001|| tt||Calibration record format
Device number
Maximum voltage
Certificate number
Reference (）
Inspector
Verifier
Indicator error [%]
Output position
Fixed wavelength UV detector center wavelength error and flat width 3.1
Center wavelength (au
Standard wavelength (a,
Center wavelength error
30 (mgx)
Total sample (
Half widthDilute the sodium dihydrogen phosphate buffer solution to the mark and shake: the maximum concentration of the solution is 1.0×106 g/ml. Then use the buffer solution to prepare 2.0×106 g/ml vitamin B solution: A. Preparation of 420 mm/s sodium dihydrogen phosphate buffer solution: Weigh 1.79 g of solid sodium dihydrogen phosphate on an analytical balance, put it into a 50 ml beaker, dilute it with distilled water, and transfer it to a 250 mm2 volumetric flask. Rinse the beaker 3 times with a small amount of sugar water, transfer the rinse solution into the volumetric flask, then dilute it with distilled water for a while, and pour it into the mouth. Reserved in the bottle, 6
Appendix B
Gas system
Voltage indication error
Current indication error
Stability
Center wavelength error
Filter half width
Wavelength indication error
Wavelength stability
Baseline drift
Baseline noise
Detection limit
Qualitative measurement repeatability
Qualitative measurement complexity
Insulation resistance
Remarks:
IJG 964—2001
Verification certificate (back) format
Appendix C
Inspected unit
Only device model
Manufacture!
Appearance inspection
Gaoyu power supply
Electric current range and indication error
Electric current indication
Output medium voltage V
Indication error/(%)
2.2Current indication error
Maximum range of battery A
Amperemeter value A
Power supply stability
Power supply stability
Wavelength indication error and repeatability
JJC964—2001|| tt||Calibration record format
Device number
Maximum voltage
Certificate number
Reference (）
Inspector
Verifier
Indicator error [%]
Output position
Fixed wavelength UV detector center wavelength error and flat width 3.1
Center wavelength (au
Standard wavelength (a,
Center wavelength error
30 (mgx)
Total sample (
Half widthDilute the sodium dihydrogen phosphate buffer solution to the mark and shake: the maximum concentration of the solution is 1.0×106 g/ml. Then use the buffer solution to prepare 2.0×106 g/ml vitamin B solution: A. Preparation of 420 mm/s sodium dihydrogen phosphate buffer solution: Weigh 1.79 g of solid sodium dihydrogen phosphate on an analytical balance, put it into a 50 ml beaker, dilute it with distilled water, and transfer it to a 250 mm2 volumetric flask. Rinse the beaker 3 times with a small amount of sugar water, transfer the rinse solution into the volumetric flask, then dilute it with distilled water for a while, and pour it into the mouth. Reserved in the bottle, 6
Appendix B
Gas system
Voltage indication error
Current indication error
Stability
Center wavelength error
Filter half width
Wavelength indication error
Wavelength stability
Baseline drift
Baseline noise
Detection limit
Qualitative measurement repeatability
Qualitative measurement complexity
Insulation resistance
Remarks:
IJG 964—2001
Verification certificate (back) format
Appendix C
Inspected unit
Only device model
Manufacture!
Appearance inspection
Gaoyu power supply
Electric current range and indication error
Electric current indication
Output medium voltage V
Indication error/(%)
2.2Current indication error
Maximum range of battery A
Amperemeter value A
Power supply stability
Power supply stability
Wavelength indication error and repeatability
JJC964—2001|| tt||Calibration record format
Device number
Maximum voltage
Certificate number
Reference (）
Inspector
Verifier
Indicator error [%]
Output position
Fixed wavelength UV detector center wavelength error and flat width 3.1
Center wavelength (au
Standard wavelength (a,
Center wavelength error
30 (mgx)
Total sample (
Half width
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