Some standard content:
Verification Procedure for Laboratory Liquid Chromatograph
JJG 705—1990
Verification Procedure for Laboratory Liquid Chromatograph
Yeriticatinn Reglatlou For Liquid Chromatograph Used tn laboratoryJJG05—1990
This verification procedure was approved by the State Technical Supervision Bureau on July 28, 1990, and was implemented on January 1, 1991: Responsible unit: National Standard Material Research Center Responsible unit: National Standard Material Research Center The units responsible for the technical provisions of this procedure are responsible for the main drafters of this procedure:
Yue Shu (National Standard Material Research Center)
Additional drafters:
Wu Bandi
(National Standard Material Research Center)
Technical requirements
Verification items
Verification items and verification methods
Verification result processing and control period
Record 1 Verification certificate (Vest) format
Thank you for recording 2 night results notification (back! Format appendix stable width certificate format
Appendix 1 standard configuration
Appendix 5 linear regression method work line
Laboratory liquid chromatography quarantine inspection procedures
This regulation guarantees the use of ten newly manufactured, used and repaired pieces of liquid chromatography-mass spectrometers with external visible light (fixed wavelength or adjustable wavelength), fluorescent markers (fixed wavelength or adjustable wavelength) and small standard light measurement instruments (hereinafter referred to as instruments with negative filters), input devices, chromatographic analysis instruments, test data and data processing equipment. Figure! Typical liquid chromatography product resistance orange diagram, treasure using sample rate in the chromatograph The difference between the distribution coefficient of the mobile phase and the attachment coefficient is determined by the market. The components are separated and tested according to the retention time and the monthly response value. The source point
flow chart
2 Technical requirements
1 Appearance
The instrument should be marked with the following: name, number, standard! Name, date! "H" series number (or serial number), etc. 1.1
1.2 The instrument should be complete and complete.
1.3 The instrument adjustment knobs, buttons, switches, etc. can work normally, and the indicator light is sensitive. 1.4 The source load, cable, etc., the joints and the index library are tightly matched. 1.5 The liquid pipeline should be made of unsawed pipes, and the joints should be tight. Within the specified range: use seven leaks. . 2 Concentration system
2.1 Flow rate setting value error S: less than, 2%5%: * Flow rate qualitative error: less than -2%-3%, 2.2 Gradient accuracy setting error: less than 3%. 3 Temperature box setting range error A: less than ·2, temperature control total integrity error 1: less than or equal to 10 (no explanation, the instrument does not test this item)
4 Fixed parts, fixed mother continent A weight belt
4.1 * Qualitative measurement repeatability error (8 times measurement) R.SF2: less than or equal to 1.5%: 4.2 Selected measurement base repeatability error (8 times measurement) R: less than 3,%5 Detector performance
5.1 Load-time optical detector
Total quantity of the control material approved by the national administration department. 1512
5.1.1 Due to the fixed wavelength ultraviolet detector, the error of the indication is less than 2Tule5.1.2 The error of the ultraviolet light filter is less than 12mn; the double difference is less than =- Inm.
# shallow drift: less than or equal to 5×1 (AL). Baseline sound: less than or equal to 510 4 (AL), 5.1.4 Minimum measurement mass (static): 410-%m (the concentration of the alcohol solution) 5.1.5 Absorbance selector error: less than or equal to +0%
5.1.6 Absorbance selector error: less than or equal to 2.0% 5.2 Optical detector
5.21 Display error: less than ten ± 5rm (due to fixed and adjustable range): 5.2.2 Intensity: 10/m The response of the dissolved acid wave on the recorder is more than 7% of the range (the detector range is small, the input voltage and the detector voltage line are shifted: less than + or equal to +S×1-3 (AU1|| tt||Linear noise: less than or equal to +5*1) (AU) Total measured concentration: 5-\ (sulfuric acid solution) 5.2.4
5.2.5Line range: 10 or equal to 1m3
5.2.6Line error due to selector change: less than or equal to 2.0%: 5.3Refraction detector
5.3.1*Sensitivity: 1 non-1g/m3Acrylic precipitation liquid has a full response of more than 70% on the recorder (when the selector is set to the minimum, the recorder input voltage is opposite to the detector output voltage) 5.3.2*Baseline drift: less than or equal to. 5×1-6 (RI1/h). Inner wire noise: less than 10 equal to ±5×1-(RILU5.3.5 Product concentration: 5×1g/m3 (propylene glycol solution)5.1.4 Loading speed ±: greater than 10,5.3.5 Range selector shift error: less than 10 or equal to 2.0%: Three verification conditions
Stone environment
Stone.I The room where the instrument is installed should be clean and free of dry and corrosive gases, and the indoor exhaust should be good. 6.2 The belt should be firmly placed on the workbench: for easy operation, without strong mechanical operation and electrical interference, and the instrument should be well grounded
0.3 The ring mirror intensity is 10-3Ut:, the temperature fluctuation within an hour does not exceed =3t (with RT detection, the temperature change does not exceed 2), and the humidity is less than 85%.
Power supply requirements
7.1 Mains voltage: 22U+22V
T.2 Power frequency: 50:0.5Hz
B Digging equipment
8.1 Stopwatch, the change value is less than 0.13, after the station is determined. Analysis day and a half, the maximum weighing 200g, the small division is 0.1, the wire inspection grid, 8.2
8.3 Wear plate: 5[J(1 1,
%.4 Zhong Kang copper thermocouple and matching temperature meter, after the determination of the content of %.5 mercury glass thermometer, 050 (centimeter: 0.1), a meaning, after the calibration of the standard 8.0 digital Y multi-calendar (5 and a half) (or digital: send table): 02001rV (the recorder used with the instrument, after the standard is modified to replace the digital Ning multimeter),
Yu.7 emitter: 10., 50l. Each purchase, according to the standard, J0ml. Two. 8.% standard substances and test examples *: war, modified quinine acid standard substances, first-class, ethanol, state and other reagents and their equivalents and For details of the preparation method, see Appendix 4.8.9. Use pure water for alcohol, HPTC, sulfur-containing agents and test fluids. 8.10
Ultraviolet absorption standard solution (solution),
Four verification items and verification methods
\Perform external inspection of the instrument according to the instructions in Sections 1.1-1.4. 1. Pressure resistance verification: Connect the infusion system, sampler, color column and detector of the energy-saving device, use methanol as the flow cabinet, and set the flow rate to [ml/mic. Start the receiver according to the instructions, keep it stable for 10 minutes, and use a filter to check that there should be no wet marks on the joints. Next, pump the pressure sensor (below the pressure sensor) to make the pressure reach 90% of the maximum allowable value, and wait for 5 minutes for the light method to be full,
11. The overall flow adjustment set value error S and flow rate specification error SR are appropriately determined. Under the experimental conditions of Article 10, read the set flow rate according to Table 1, keep the flow constant, collect the mobile phase in a pre-cleaned and weighed container bottle at the mobile phase outlet, and use a stopwatch to accurately collect 1U-25 minutes, weigh, and calculate 5k and S according to formula (1) and formula (2): S = (Pm-F/Fx 0%
Sk - (Fmx - Fm)/FX 100%
Where: Flow rate setting value difference (poly); F.- -{W2- W,)/o,, Flow time measured value (rn_/tair) W - Weight of mobile phase in volumetric flask (?:
W - Density of mobile phase at actual temperature (g/e); Time for collecting mobile phase [n);
S - - Error of stability of flow (%)
Fm - Maximum value of flow display in same-distance measurement (ml.m.n) mm-E steel minimum value mL/mn): the same group of measured values of the calculation of the cooking level (nl/min) 12 constant temperature box temperature agreed value makes the heart and the temperature control error, the difficulty of determination, (1)
non-constant temperature box has a hole to capture the temperature meter: the thermometer can be fixed in the box, this method is used for fixing. Column box without holes, the thermocouple can be fixed in the column box (the cold end is under the word), the lead wire is connected to the measuring instrument, the column box door is closed, the lowest controllable temperature (usually room temperature 7) is selected and the maximum range of the whole group is known. The temperature is set at two points, the control instrument is operated, and the temperature is raised. Wait for the indicator to stabilize, record the increase or decrease on the measuring meter, record once every minute, and the meter? In order to calculate the correlation between the arithmetic mean, the fixed value and the average value, the difference between the maximum and minimum values of the 7 measurements is the temperature control stable error T.
Quantity determination ()
*
Yi Ji said standard time (i)
Allowable error section
Table 1. The maximum value of the fixed value can be collected according to the actual price of the machine. Since the sequence is limited to random selection, the monthly limit is not set. The total reading is limited to one second. The film is a small amount of mobile phase, etc., which is to be verified by the most secret film for 5 minutes. The mobile phase can be collected, and the accuracy of the gradient program can be changed through the control device. The mobile phase is water, and the total mobile phase is liquid containing water. A must be passed from 100% to U, and the mobile phase must pass through the positive baseline (the potential phase does not pass through the chromatographic column) with A. After starting up, only the recorder is used. After the light is flat, record the readings on the recorder, use the calculator to calculate the weights, and record the "comparative signal value: the output signal value: the potential pressure executes the gradient program, the gradient line changes, and the output signal of the various mobile phases is read in detail. Record the readings. Repeat the measurement twice, calculate the average value, and record the above content and the corresponding input signal. Calculate the accuracy of the value, and take the maximum value as the instrument error. I6
Where:
1st stage gradient hysteresis accuracy (%);
1st stage input signal or record only the deviation number: each section output signal or record the instrument reading translation value P
Figure 2 Accurate control of gradient flow
Qualitative measurement of the quality
Connect the instrument well and make it work normally. Use a microliter syringe (preferably a quantitative tube) to inject a standard solution (tea, decoction, etc. for UV-visible detector; ruthenium for fluorescence detector; pyrolysis for refractometer detector) or a stable sample to be analyzed. Record the solution time and peak product. Select the number of consecutive measurements and calculate the relative standard deviation RS according to the formula (RST)
2(x, - x\xn - 1) x
RS is the relative standard deviation of qualitative and quantitative measurements. Wu: x
The first: The peak product of the measured value; the result of the first measurement:
Measurement number:
Number of measurements:
15 UV-visible light detection performance calibration 15,1 The calibration of the detector wavelength is called fixed wavelength. The UV transmission band is usually obtained by a piece of film to obtain light of a fixed wavelength, and the light source can be carefully filtered to obtain the light. 15.2 Adjustable wavelength - A visible light detector with small wavelength difference. Connect the detector to the recorder, connect the power supply to the preset point and after it is stable, use the injection pipe to inject the UV and standard wavelength and reference solution into the sample area and Ruby cell of the detector, rinse the net, and then fill the two chambers with: UV standard solution (235nm, 257mm, 315mm and 35mm) according to the standard wavelength (235nm, 257mm, 315mm and 35mm) of the UV standard solution. (mm) To verify the wavelength indication error of the instrument, adjust the recording paper to 4mm/min, lower the detection wavelength to 5:m lower than the standard solution (for example, at 25°C, the detector wavelength is first set to 252nm), adjust the recording pen to the intermediate position, and then change the wavelength from 252mr to 262u in 15 seconds. Draw the curve of Figure 3 on the recorder. The difference between the wavelength of the most accurate (through the most six!) and the marked wavelength is the wavelength indication error. Use the same method to determine other points and re-measure each point. 3 times, the difference between the maximum and minimum values of the lamp wavelength is the wavelength error
15.3 Detection of line drift and baseline noise
Connect the instrument according to the manual, and select the following experimental conditions: external absorption is 254: mobile phase is 100% methanol: flow rate is 1.0mmin; Taypica cell is air: absorbance is selected as the range of absorption; recording paper is 5-10rmi, turn on the machine and wait for the baseline to be determined, record the baseline for 30-40 minutes, and calculate the noise of the line source drift. , 242
Figure 3 The error of the digital indication is the main error of the light 15.4 Detection of the small detection range
In a static state, inject 4×-10% methanol solution with a syringe, and select the sample with a height greater than or equal to the baseline sound peak. According to formula (5), the minimum detection range Gi = 2-HN+ -/H
Wherein:
Minimum detection degree ():
H—noise peak height (recorder grid number or measured height cm) r group sample concentration (g/rl);
H—sample peak height (recorder path number or measured height n), 15.5 line ratio range calibration
Reverse the detector recorder, connect the single core, use 2% benzyl alcohol aqueous solution as the acetone solution, propylene glycol-2% isopropanol series aqueous solution as the filter, the ultraviolet absorption wavelength is 2541m, rinse the absorbent ten times with the intermediate solution under static state, after the recorder indicator is set, adjust the recorder to zero, according to the lack of .[%, .2 music, ..1. heart% limit -2% isopropanol acetone solution and fill the filter, while recording the readings of each filter. Repeat 3 times , take the technical average: 1546
reverse the content-data collection and value film, find the user curve point (the reading is more than 5% of the theoretical value), this is the upper limit of the line range "h, according to formula (5) to calculate the acetone range c, value, out, (accurate acetone) calculate the detector performance range of 15.6 absorbance selector compensation error calibration
at the output end of the detector only connect a digital meter (or directly with the instrument matching the old recorder that has been calibrated, the instrument with the absorbance display function does not need this multi-currency meter), under the normal working condition of the instrument: connect a selector, read the non-correlated potential value on the digital recorder or the absorbance on the display, the car is measured for times, take the average value, calculate the multiplication error of two adjacent gears H, take H. The maximum position represents the gear shift error. H, - xY Y + 100%
Wherein: X is the first mark;
Y is the first selector! Test agent recorder or digital meter, 16. Test of fluorescence test data performance
16.1 Test of indication error of fixed wavelength optical detector
Because the fixed wavelength optical detector has two filters, they can be removed and put on the forbidden filter. The adjustable wavelength optical meter is called the reference temperature method of paragraph 15.2 (the instrument is used normally, so it is not tested today) 16.2 Test of baseline drift and baseline port Connect the test filter to the recorder, and after the instrument is preheated, use the emitter to put the acrylic and water (about 5) into the dynamic pool ( Start with a small burning plate at the entrance), re-rinse the pool clean, then inject 5ml of acetone, after 11 minutes, inject 5ml of 15ul/h H2O solution (be careful not to have moisture), select the sensitivity setting, record for 30 minutes, and calculate the acoustic base drift (the recording paper speed is 10mm) ir:in)e
16.3 Sensitivity and quality test. Connect the detector to the recorder, select the sensitivity setting, the excitation wavelength is 345, and the emission wavelength is 455m. Use a syringe to slowly inject 30% H2O into the flow cell. Connect the power supply. After a few minutes, the recorder will start to work. Adjust the zeroing knob to make the recorder or pen at the same point as the recording paper. Then use the injector to inject 10u/ml of U.05ruA of 10u/ml of 1% thiocyanate into the flow cell. The recorder should be at the 70% position. Calculate the detector sensitivity and then calculate the minimum detection concentration according to the formula = 2·HN·c/H (the meaning of each symbol is the same as that of formula (5). 6.4 Standard calibration of the standard 16.3 of the standard. In this case, use the syringe to inject 0.05rxl of HSC aqueous solution into the flow cell. Wash the cell and then drain it into the flow cell according to the decision. Then, add 1×10-, 2×5-, 3×10-1g/ml of 1% thiocyanate aqueous solution of H0. Record the recorder data at the same time.Take the arithmetic mean value for 3 times, and plot the total defect of sieve acid and the reading of the recorder. Find the damage point of the curve (the reading is 5% lower than the theoretical value). This point is the upper limit of the load capacity. In Section 16.3, the value of "/c" is obtained, the ratio is linear, and the range selection is 16.5. The calibration frequency of the shift error is performed, and the calculation method is the same as in Section 15.6. 17.1. Calibration of baseline source and baseline noise. 17.2. After the detector and other external devices are connected, connect the source and heat it: use pure water as the mobile phase, the flow rate is 1 meter, and the reference is filled with pure water. The system is selected at the minimum gear. The benzene line is recorded for 3 minutes, and the benzene line drift is calculated. t$47
and the acoustic wave of the device are maintained (pay special attention to the temperature fluctuation in the experiment). 17.2. The sensitivity and minimum detection concentration of the light detection are removed from the chromatographic device. After rinsing the sample pool with steamed water for many times, wash it 3 times, select the most sensitive range, and make sure that the instrument input voltage is the same as the tester output voltage. Adjust the recorder to 0. Use a diffuser to inject 10" g/m3 liquid into the sample pool. The recorder should be at a position above 70% of the full range. Repeat 3 times and take the arithmetic mean. The baseline measured in Section 17.1 is obtained by using the minimum concentration measured by equation (5): 17.3 Test for the corresponding instrument
After the sample pool and the sample pool are rinsed with water 3 times: fill the pool with 105, 10-1, 10, 2×101, 310, 4×10-1, 5×10-g/ml alcohol-water liquid in turn, and record the recorder reading at the same time. Plot the concentration and the recorder reading to find the inflection point (the reading is 5% lower than the theoretical value). This point is the upper limit of the linearity. The value of c in Section 17.2 is the linear range. 17.4 Test for selector shift error
The operation and calculation methods are the same as those in Article 15.6. Note: All chromatographic columns used in the calibration are (reversed phase) 5. Calibration results processing and calibration period
18. According to the provisions of this regulation, if at least the calibration items marked with * meet the specified technical indicators, the instrument is a qualified instrument and a calibration certificate will be issued:
indicates that an item marked with * is unqualified. If it is a detector, a certificate of qualification can be issued, but it should be noted that the test is unqualified. If the other items are unqualified, the instrument is an unqualified instrument. If the technical indicators are not met, a calibration result notice will be issued. 19. The calibration period of laboratory chromatographs is tentatively set at two years. If parts are replaced or there is doubt about the performance of the instrument: it should be accompanied by
Appendix Calibration Certificate [Back] Format
Control Results
, please
2. + machine:
·RST+
, grid divider:
: the longer the indication, the more:
wavelength indication difference
x baseline environment by
·benzene play evaporation
primary school Xie concentrated store
selector call Xie requested
*baseline source change
*minimum addition to the problem seat
E, conclusion:
sexual change:
electrical manufacturing
on the wide aybZxz.net
sexual solid
*limited small inspection double heat
Selector recovery error
Selector speed error
Appendix 2 Calibration result notice [back] format Calibration result
Describe the actual situation of the inspection: find the solution and solve the problem
1. Appearance inspection
Calibration record format
Appendix 3
Or inspection model Phase chromatograph calibration record
F5 number
2. Pump trace volume setting reading error and flow stability error Determine the withstand pressure (Ma)
tw,-w /p
shenyang dynamic box
actual measurement method
3. Gradient accuracy verification
B change the change l
. The value of the value box temperature setting value change the efficiency control stability verification only
5. Qualitative and quantitative measurement of egg female verification
sample name
shennan time
shrimp area
6. Combined with the visible flow detection data performance control
river length worst
resistance to secretion pump rotation
small amount of detection Huan Chen (tea:
within (%
257mam
model map: guide
method length west map
basic net production
minimum detection to gradual pressure (within:
micro eye reading
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.