Some standard content:
Verification procedures for gas chromatographs
JJG 700—1999
Verification procedures for gas chromatographs
Verification of gas chromatographs
Cian Chrmatkgraph
JJG 70H—1999
Generation G7009m
..---+.+
This standard was approved by the State Administration of Quality and Technical Supervision on May 14, 1999, and was implemented on September 1, 1999. Responsible unit: National Physical and Chemical Technical Committee Drafting unit: National Standard Material Research Center This standard is entrusted to interpret the provisions of this standard. Drafting person: Jin Meilan (National Standard Material Research Center)
Technical requirements
Verification policy
4 Verification items and determination methods 5. Processing of calibration results and period of use. Appendix A. Calibration of micro-emitters. Appendix A. Positive value of daily gas flow rate. Appendix B. Calibration certificate and calibration results. Appendix C. 1 (Back) Format. Appendix C. Calibration record of gas chromatograph. Calibration procedures for gas chromatographs. Calibration procedures for gas chromatographs are applicable to new, regular and peak-treated instruments. (1) Calibration of flame ionization (F[I), flame light change (non-ionization, electron capture, phosphorus [as detectors) for general laboratory gas detectors. Micro-ionization and ionization detectors can refer to the flame ionization detector calibration method for the test piece. |tt||The gas sample (hereinafter referred to as the gas spectrum) is a kind of chromatography. The gas sample is vaporized by the carrier gas and brought into the chromatograph for separation. The sample is then selected and tested by the instrument. The components are characterized according to their minimum retention time and response value. The analysis is carried out. The gas path system, fiber inlet system, chromatograph, outlet system, detection system, memory or whole processing system are composed.
2 Technical requirements
Technical indicators
2.1.1 Pre-production of the chamber temperature of the instrument for qualitative, repeatable and accurate determination of the components The operation sound, base shift, sensitivity or measurement limit should all be in accordance with the requirements of the data sheet, and the stability of the gas flow rate should be checked regularly, and the instrument should be tested for the error items H. The technical indicators in Table 1 of this specification should be checked regularly.
Table 1 The main technical indicators of the gas spectrometer
should be determined and compared with the actual gas color determination
(Inmm)
smoothness determination
baseline purity
baseline source (Mirnin;
no*
quantitative film
memory temperature difference
llmVdr
1× [0 \g +]-
The technical specifications of the instrument during use and after repair shall meet the requirements of this specification.
3 Verification conditions
3.1 Verification environment and instrument installation requirements
3.1.1 Verification environment
3.1.1.1 Ambient temperature: 5℃--35℃
3.1.1.2 Relative humidity: 20%-85%. 3.1.1.3 Flammable and explosive materials related to actual light shall not be stored in the environment. 3.1.2.1 Gas pipelines should use stainless steel pipes, polypropylene pipes, nylon pipes, and rubber press equipment. 1 Stopwatch: graduation value 0.01, syringe: range 10. Need accurate numbers, more calibration methods, Appendix A. Air meter: measurement range 800u-[060HTz, micro uncertainty 2.0 Flowmeter: full scale uncertainty 1%
Platinum resistance thermometer: Pt100) accuracy 0.3t: Digital multimeter: voltage measurement uncertainty variable SuV, electric attachment measurement uncertainty U.4 (current [mA), variable chromatograph calibration special measuring instrument.
3.3 Standard material research
Benzene-methyl alcohol solution;
Hexadecane-isooctane solution;
Medium-base phosphorus·eutrophil solution;
Endomeric hexadecane-isooctane solution;
Ural phosphorus·isooctane solution: 3.3.f (hydrogen) medium methane standard gas. 3: It should be able to use the national metrology department approved by the national metrology department, and the unit that has a manufacturing license of 3 years of metrology instruments should provide the standard.
4 Verification items and verification methods
4.1 General inspection
4.1.1 The instrument should have the following information: instrument name, model, manufacturer name, factory date and factory number, and the national standard instrument should have the manufacturing license mark of metrology instruments. 42 Under normal working conditions, use the leak test liquid to check all gas-passing joints from the gas source to the instrument, and there should be no leakage. 4.1.3 All parts of the rotation, button, switch and lamp are working properly. 4.2 Check on gas flow rate stability
Select an appropriate carrier gas flow rate, and after it is stable, use a flow meter to measure it, and measure it for 6 times in a row. The relative deviation of the average value should not be greater than "%.
4.3 Source inspection
4.3.1 Check on temperature stability of the box
Connect the connection line of the offset current flow meter to the digital meter (measurement instrument for color drop test) to 1, then fix the probe of the thermometer in the middle of the box, set the machine temperature to 70℃, heat it, and wait for the group to become more stable. Observe for 10min, record the change every time, and calculate the temperature. The temperature difference corresponding to the maximum and minimum values in the mathematical table is calculated by comparing the difference with the arithmetic mean of the internal temperature measured in 1Un, which is the qualitative value of the box temperature. 4.3.2 Program temperature rise test room
Follow the test conditions and test methods of 4.3.1 to carry out program temperature rise test. Select the initial temperature 7: and the final temperature 2:. The heating rate is 1:n. The initial temperature is stable: the program temperature is raised, and the number of times per minute is recorded until the final temperature stabilizes. This is repeated 2-3 times to get the maximum deviation of the corresponding point, and the result should be adjusted according to the formula:
deviation = (m (0 10)%
Wherein: y—maximum temperature of corresponding points [7]; m—average temperature of corresponding points (7):
average absorption temperature of corresponding points ()
4.4 Attenuator error verification
Under the conditions of the detection of the detector properties, check the error of the attenuator corresponding to the detector. After the instrument is stable, connect the signal output end of the detector to a digital multimeter (or chromatograph for special measurement). When the error is 1, measure two electrical values and then set the range to 2. , 4, 8.… from the maximum gear actually used, measure the base voltage, the error of the adjacent second gear should be less than 1%,
4.5\TCD performance verification
4.5.1 Verification components see Table 2
4.5.2 Baseline elasticity and baseline source shift verification
According to the verification conditions in Table 2, select the sensitive gear, set the bridge current or thermal end, after the special baseline is set, adjust the output signal to the middle of the recording chart display, record the line reduction ratio, measure and calculate the baseline sound and baseline 1.5.3 Desensitization test
According to the specific purpose of the instrument, it can be calibrated according to 4.5.3.1 or 4.5.3.2. 4.5.3.1 Verification with liquid standard substances
Follow the verification conditions in Table 2. After the base residue is stable, use a calibrated microsyringe to inject 1-2 ml of benzene solution with a concentration of 5 g/mL, and select samples 6 times in reverse order. Record the extraction surface. 4.5.3.2 Verification with gas standard substances
Follow the verification conditions in Table 2 Verification conditions: inject 1 mol/mo CH/N, 1 lTi or (TL/He standard gas, and continue to invert the sample, and record the methane amplitude.
4.5.3.3 Calculation of sensitivity
Wu Xiao: S
TCD sensitivity (mVmi/mg):
Arithmetic mean of the peak or methane peak product (mV-un)W——* or methane injection (see ():
: Calibration film or gas flow according to al)
09 - n
Clean and safe
( 3091
22 94:
(mn/) For slower speed, see Appendix B.
When the pump light is used to record the peak and integrate, the width of the single peak of the methane screen is not less than 5mr, and the height is not less than 60% of the peak compensation of the recorder period. (2) The peak front! 4 According to (3) I calculate A 1.6SG,G,A,K
wherein: A is the product of benzol or methane (nVmin); C is the sensitivity of the recorder [mV/cm]; C is the efficiency of the recorder paper [nsinm];
is the arithmetic mean of several measured peak areas (m): K is the multiple.
4.6FID performance verification
4.6.1 The verification conditions are shown in Table 2.
4.6.2 Verification of baseline drift of line media
According to the verification conditions in Table 2, select and calibrate the sensitivity, and after the base is stable, adjust the "output signal to record the whole product display diagram", record for half an hour, and measure the baseline noise drift. 1.3.6 Detection limit determination
According to the specific application, the determination can be carried out by method 4.6.3.1 or 4.6.3.2. 4.6.3.1 Verification with liquid standard material
The verification conditions in Table 2 are guaranteed. In the state of tracking, after the base load is stable, use a microinjector to inject 1-2ul of a 1 μmol or 10 μmol/l n-decane half-solution with a concentration of 6 times, and record the peak area of n-hexadecane.
4.6.3.2 Determination with gas standard mass
According to the test conditions in Table 2, inject 10 μmol/wl CH/N standard gas, and inject 6 times continuously, and record the peak area of n-hexadecane
Calculation of detection limit
Where: Tm
FI1) Detection limit (g):
N-baseline peak (A);
WThe injection volume of hexadecane or n-hexadecane (g): A—arithmetic mean value of alkane or alkane diol (A4.7 FPD performance verification
4.7.1 Verification conditions see Table 2.
4.7.2 Base or taste and baseline drift verification. According to the verification conditions in Table 2, the measurement method is the same as that in 4.6.2. 4.7.3 Detection limit verification
According to the specified conditions in Table 2, put the instrument in the most stable state, wait for the base level to stabilize, inject the solution of formazan-free ethanol with a concentration of [0m], inject 1l-2l, and send the sample 6 times in a row, record the peak area of the current or phosphorus
+.7.4 Detection limit output
In:
12:Wnsj
to the magnetic cell limit (
star line music (mV):
phosphorus peak surface arithmetic mean (rVs): methyl disulfide bomb injection scale ();
avoided peak quotient [mV]:
the peak cage at 1A of the system (
the front atom in the molecule is the base pair of the sparse atoms in the molecule
the base pair of the sparse molecules in the molecule is the base pair of the sparse molecules in the molecule. The base pair mass Tp
26.124.118
4.BECD Performance range
4.8.1 Test conditions 52
4.B.2 Line media 11 and baseline drift specifications
According to the test conditions in Table 2, select the frequency sensitivity gear, adjust the output signal to record the graph or only display a small part of the graph, after the compensation, record the average value for 24 hours. Calculate the baseline drift and baseline source drift, 4.8.1 Detection limit test
According to the test conditions in Table 2, make the receptor at the maximum temperature, after the line and the wall are stable, use a microinjection to inject 30.1 package of internal 666-external rate solution, inject 1~2u, inject 6 times continuously, record as the internal 666 4.8.4 Detection limit calculation: Pw\
C Detection limit (:
H Line noise (nV):
C Sample injection temperature ():
A Arithmetic compensation of the 666 peak machine (mVrin):
4.9 MFLI performance test:
4.9.1 Control conditions see Table 2. 4.9.2 Line noise and source effect: According to the conditions in Table 2, select the type and appropriate attenuation. When the baseline is stable, record the new line. Measure and calculate the baseline median and line drift.
4.9.3 Detection limit verification: See Table 2. Verification conditions: Select a suitable test chamber, use the most accurate camera to inject 10m5/L of isooctylphosphine-isooctanoate at 12°C for 6 times, calculate the arithmetic mean of the peak areas of isooctylphosphine (or isooctylphosphine), 4.9.4 Calculation of the total molar mass of nitrogen contained in the injected sample (w/w): 1-10 atoms of nitrogen, the arithmetic mean value is: w/w = 2 × 14 = 0.154 atoms of nitrogen, or w/w = 2 × 14 = 0.154 atoms of nitrogen. The peak area of the wine is the same as the value of the final product:
and the night energy is the same as the original 331
the correct quality of the wine
4.10 Quantitative reproducibility test
The relative standard deviation R of the peak area measurement is expressed as follows: a
Relative standard deviation (%):
Number of measurements:
The area measured for the first time;
Work——the peak area of n injections is calculated as the average value; i Sample number.
5 Verification result processing and verification cycle
×100%
5.1 Verify the products that do not meet the technical indicators in Table 1 according to the requirements of this procedure. A calibration certificate shall be issued to qualified instruments, and a calibration report shall be issued to unqualified instruments. 5.2 The calibration period of gas chromatograph is 2 years. Appendix A Calibration of microinjection device The microinjection device has good airtightness and should be cleaned and dried before calibration. The water used for calibration should be clean. Calibration method: At room temperature, draw a certain volume of water and cover the needle with a silicone rubber pad. Weigh it on an analytical balance of ten-thousandths of a gram. Then draw out the mercury and weigh it again. The mass of mercury can be obtained by subtraction, and then the actual volume (ml) is calculated according to the following formula: Formula A: V M——The mass of the first weighing (); |The mass of the second weighing (g);
The density of mercury at room temperature (n:l
Each volume point is calibrated 6 times and the arithmetic half mean is taken. The relative standard deviation is within 1%. Appendix H Correction of the rectified gas flow rate
The gas flow rate measured at the detector outlet is corrected by the following formula F,-iF.
Corrected carrier gas flow rate (nl/mun):
Carrier gas flow rate out of the detector measured by soap film flowmeter at room temperature (called): Temperature (K):
Wetness (K:
Saturated vapor pressure of water at room temperature (MPa): Atmospheric pressure (Ma):
Pressure correction factor.
×(p.- po)*
(p pu -
Formula: Note: Base strength (Ma):
Verification certificate and verification result notice] Format Appendix
Verification result
Detector name
Flow rate stability
Box temperature stability
Program temperature rise stress
Base noise
Line displacement
Test instrument replacement error
Appendix: Verification record of gas analyzer
Light unit
Submit to control monoclonal antibody
Money department
After the hair is in place
Night instrument number
Received R period
1 .External measurement:
2.Carrier gas liquid speed qualitative: (m/in)
3.Detection end name:
2.Verification conditions:
Color low +1
Production space repair
Remember tea drop sensitivity seat
Second class
5.Wet stability in the box:
6.Program temperature rise single complex:
7, some money throat sound
8.Line depth shift:
9, Grade high peak surface class:
10.Replacement of reducer to eliminate recognition error:
11.Color latent map number:
12, Preparation:
Brush manufacturing!
Atmospheric F
Test product
Detector pressure
Standard item standard
Single mean value
27 (%)2 Verify baseline noise drift
According to the verification conditions in Table 2, select the appropriate sensitivity, and after the baseline is stable, adjust the "output signal to record the whole product display diagram", record for half an hour, and calculate the baseline noise drift. 1.3.6 Determination of detection limit
According to the specific application, the determination can be carried out by method 4.6.3.1 or 4.6.3.2. 4.6.3.1 Verify with liquid standard material
According to the verification conditions in Table 2, keep the calibration state, and after the baseline is stable, use a micro-injection to check the concentration of 1-2ul, with a concentration of 1mn 4.6.3.2 Using gas standard for determination According to the test conditions in Table 2, introduce 10 μmol/wl CH/N standard gas, and continuously inject 6 times, and record the peak area of hexadecane. Calculation of detection limit Where: Tm 1) Detection limit (g): N-baseline peak (A); Injection amount of hexadecane or hexadecane (g): A-arithmetic mean of hexadecane or hexadecane peak (A4) .7 FPD performance verification
4.7.1 Verification conditions are shown in Table 2.
4.7.2 Baseline sound and baseline drift verification. According to the verification conditions in Table 2, the detection method is the same as in 4.6.2. 4.7.3 Detection limit verification
According to the specifications in Table 2, put the instrument in the most stable state, wait for the base level to stabilize, inject the solution of 100M formazan-free ethanol with a concentration of 10M, inject 1l-2l, and repeat 6 times, record the peak area of the current or phosphorus
+.7.4 Detection limit output
Insert:
12: Wnsj
to the magnetic cell limit (
star line music (mV):
phosphorus peak surface arithmetic mean (rVs): methyl disulfide bomb sampling scale ();
avoided peak quotient [mV]:
the peak cage at 1A of the system (
the front atom in the molecule is the base pair of the sparse base
the base pair of the sparse molecule is the base pair of the sparse molecule. The base pair mass of the base pair is
26.124.118
4.BECD Performance range
4.8.1 Test conditions 52
4.B.2 Line media 11 and baseline drift specifications
According to the test conditions in Table 2, select the frequency sensitivity gear, adjust the output signal to record the graph or only display a small part of the graph, after the compensation, record the average value for 24 hours. Calculate the baseline drift and baseline source drift, 4.8.1 Detection limit test
According to the test conditions in Table 2, make the receptor at the maximum temperature, after the line and the wall are stable, use a microinjection to inject 30.1 package of internal 666-external rate solution, inject 1~2u, inject 6 times continuously, record as the internal 666 4.8.4 Detection limit calculation: Pw\
C Detection limit (:
H Line noise (nV):
C Sample injection temperature ():
A Arithmetic compensation of the 666 peak machine (mVrin):
4.9 MFLI performance test:
4.9.1 Control conditions see Table 2. 4.9.2 Line noise and source effect: According to the conditions in Table 2, select the type and appropriate attenuation. When the baseline is stable, record the new line. Measure and calculate the baseline median and line drift.
4.9.3 Detection limit verification: See Table 2. Verification conditions: Select a suitable test chamber, use the most accurate camera to inject 10m5/L of isooctylphosphine-isooctanoate at 12°C for 6 times, calculate the arithmetic mean of the peak areas of isooctylphosphine (or isooctylphosphine), 4.9.4 Calculation of the total molar mass of nitrogen contained in the injected sample (w/w): 1-10 atoms of nitrogen, the arithmetic mean value is: w/w = 2 × 14 = 0.154 atoms of nitrogen, or w/w = 2 × 14 = 0.154 atoms of nitrogen. The peak area of the wine is the same as the value of the final product:
and the night energy is the same as the original 331
the correct quality of the wine
4.10 Quantitative reproducibility test
The relative standard deviation R of the peak area measurement is expressed as follows: a
Relative standard deviation (%):
Number of measurements:
The area measured for the first time;
Work——the peak area of n injections is calculated as the average value; i Sample number.
5 Verification result processing and verification cycle
×100%
5.1 Verify the products that do not meet the technical indicators in Table 1 according to the requirements of this procedure. A calibration certificate shall be issued to qualified instruments, and a calibration report shall be issued to unqualified instruments. 5.2 The calibration period of gas chromatograph is 2 years. Appendix A Calibration of microinjection device The microinjection device has good airtightness and should be cleaned and dried before calibration. The water used for calibration should be clean. Calibration method: At room temperature, draw a certain volume of water and cover the needle with a silicone rubber pad. Weigh it on an analytical balance of ten-thousandths of a gram. Then draw out the mercury and weigh it again. The mass of mercury can be obtained by subtraction, and then the actual volume (ml) is calculated according to the following formula: Formula A: V M——The mass of the first weighing (); |The mass of the second weighing (g);
The density of mercury at room temperature (n:l
Each volume point is calibrated 6 times and the arithmetic half mean is taken. The relative standard deviation is within 1%. Appendix H Correction of the rectified gas flow rate
The gas flow rate measured at the detector outlet is corrected by the following formula F,-iF.
Corrected carrier gas flow rate (nl/mun):
Carrier gas flow rate out of the detector measured by soap film flowmeter at room temperature (called): Temperature (K):
Wetness (K:
Saturated vapor pressure of water at room temperature (MPa): Atmospheric pressure (Ma):
Pressure correction factor.
×(p.- po)*
(p pu -
Formula: Note: Base strength (Ma):
Verification certificate and verification result notice] Format Appendix
Verification result
Detector name
Flow rate stability
Box temperature stability
Program temperature rise stress
Base noise
Line displacement
Test instrument replacement error
Appendix: Verification record of gas analyzer
Light unit
Submit to control monoclonal antibody
Money department
After the hair is in place
Night instrument number
Received R period
1 .External measurement:
2.Carrier gas liquid speed qualitative: (m/in)
3.Detection end name:
2.Verification conditions:
Color low +1
Production space repair
Remember tea drop sensitivity seat
Second class
5.Wet stability in the box:
6.Program temperature rise single complex:
7, some money throat sound
8.Line depth shift:
9, Grade high peak surface class:
10.Replacement of reducer to eliminate recognition error:
11.Color latent map number:
12, Preparation:
Brush manufacturing!
Atmospheric F
Test product
Detector pressure
Standard item standard
Single mean value
27 (%)2 Verify baseline noise drift
According to the verification conditions in Table 2, select the appropriate sensitivity, and after the baseline is stable, adjust the "output signal to record the whole product display diagram", record for half an hour, and calculate the baseline noise drift. 1.3.6 Determination of detection limit
According to the specific application, the determination can be carried out by method 4.6.3.1 or 4.6.3.2. 4.6.3.1 Verify with liquid standard material
According to the verification conditions in Table 2, keep the calibration state, and after the baseline is stable, use a micro-injection to check the concentration of 1-2ul, with a concentration of 1mn 4.6.3.2 Using gas standard for determination According to the test conditions in Table 2, introduce 10 μmol/wl CH/N standard gas, and continuously inject 6 times, and record the peak area of hexadecane. Calculation of detection limit Where: Tm 1) Detection limit (g): N-baseline peak (A); Injection amount of hexadecane or hexadecane (g): A-arithmetic mean of hexadecane or hexadecane peak (A4) .7 FPD performance verification
4.7.1 Verification conditions are shown in Table 2.
4.7.2 Baseline sound and baseline drift verification. According to the verification conditions in Table 2, the detection method is the same as in 4.6.2. 4.7.3 Detection limit verification
According to the specifications in Table 2, put the instrument in the most stable state, wait for the base level to stabilize, inject the solution of 100M formazan-free ethanol with a concentration of 10M, inject 1l-2l, and repeat 6 times, record the peak area of the current or phosphorus
+.7.4 Detection limit output
Insert:
12: Wnsj
to the magnetic cell limit (
star line music (mV):
phosphorus peak surface arithmetic mean (rVs): methyl disulfide bomb sampling scale ();
avoided peak quotient [mV]:
the peak cage at 1A of the system (
the front atom in the molecule is the base pair of the sparse base
the base pair of the sparse molecule is the base pair of the sparse molecule. The base pair mass of the base pair is
26.124.118
4.BECD Performance range
4.8.1 Test conditions 52
4.B.2 Line media 11 and baseline drift specifications
According to the test conditions in Table 2, select the frequency sensitivity gear, adjust the output signal to record the graph or only display a small part of the graph, after the compensation, record the average value for 24 hours. Calculate the baseline drift and baseline source drift, 4.8.1 Detection limit test
According to the test conditions in Table 2, make the receptor at the maximum temperature, after the line and the wall are stable, use a microinjection to inject 30.1 package of internal 666-external rate solution, inject 1~2u, inject 6 times continuously, record as the internal 666 4.8.4 Detection limit calculation: Pw\
C Detection limit (:
H Line noise (nV):
C Sample injection temperature ():
A Arithmetic compensation of the 666 peak machine (mVrin):
4.9 MFLI performance test:
4.9.1 Control conditions see Table 2. 4.9.2 Line noise and source effect: According to the conditions in Table 2, select the type and appropriate attenuation. When the baseline is stable, record the new line. Measure and calculate the baseline median and line drift.
4.9.3 Detection limit verification: See Table 2. Verification conditions: Select a suitable test chamber, use the most accurate camera to inject 10m5/L of isooctylphosphine-isooctanoate at 12°C for 6 times, calculate the arithmetic mean of the peak areas of isooctylphosphine (or isooctylphosphine), 4.9.4 Calculation of the total molar mass of nitrogen contained in the injected sample (w/w): 1-10 atoms of nitrogen, the arithmetic mean value is: w/w = 2 × 14 = 0.154 atoms of nitrogen, or w/w = 2 × 14 = 0.154 atoms of nitrogen. The peak area of the wine is the same as the value of the final product:
and the night energy is the same as the original 331
the correct quality of the wine
4.10 Quantitative reproducibility test
The relative standard deviation R of the peak area measurement is expressed as follows: a
Relative standard deviation (%):
Number of measurements:
The area measured for the first time;
Work——the peak area of n injections is calculated as the average value; i Sample number.
5 Verification result processing and verification cycle
×100%
5.1 Verify the products that do not meet the technical indicators in Table 1 according to the requirements of this procedure. A calibration certificate shall be issued to qualified instruments, and a calibration report shall be issued to unqualified instruments. 5.2 The calibration period of gas chromatograph is 2 years. Appendix A Calibration of microinjection device The microinjection device has good airtightness and should be cleaned and dried before calibration. The water used for calibration should be clean. Calibration method: At room temperature, draw a certain volume of water and cover the needle with a silicone rubber pad. Weigh it on an analytical balance of ten-thousandths of a gram. Then draw out the mercury and weigh it again. The mass of mercury can be obtained by subtraction, and then the actual volume (ml) is calculated according to the following formula: Formula A: V M——The mass of the first weighing (); |The mass of the second weighing (g);
The density of mercury at room temperature (n:l
Each volume point is calibrated 6 times and the arithmetic half mean is taken. The relative standard deviation is within 1%. Appendix H Correction of the rectified gas flow rate
The gas flow rate measured at the detector outlet is corrected by the following formula F,-iF.
Corrected carrier gas flow rate (nl/mun):
Carrier gas flow rate out of the detector measured by soap film flowmeter at room temperature (called): Temperature (K):
Wetness (K:
Saturated vapor pressure of water at room temperature (MPa): Atmospheric pressure (Ma):
Pressure correction factor.
×(p.- po)*
(p pu -
Formula: Note: Base strength (Ma):
Verification certificate and verification result notice] Format Appendix
Verification result
Detector name
Flow rate stability
Box temperature stability
Program temperature rise stress
Base noise
Line displacement
Test instrument replacement error
Appendix: Verification record of gas analyzer
Light unit
Submit to control monoclonal antibody
Money department
After the hair is in place
Night instrument number
Received R period
1 .External measurement:
2.Carrier gas liquid speed qualitative: (m/in)
3.Detection end name:
2.Verification conditions:
Color low +1
Production space repair
Remember tea drop sensitivity seat
Second class
5.Wet stability in the box:
6.Program temperature rise single complex:
7, some money throat sound
8.Line depth shift:
9, Grade high peak surface class:
10.Replacement of reducer to eliminate recognition error:
11.Color latent map number:
12, Preparation:
Brush manufacturing!
Atmospheric F
Test product
Detector pressure
Standard item standard
Single mean value
27 (%)2. Use gas standard for sensitive quality determination. According to the test conditions in Table 2, introduce 10 μmol/wl CH/N standard gas, sample 6 times continuously, and record the peak area of hexadecane. Calculation of detection limit: Tm/FI1) Detection limit (g): N-baseline peak (A); Injection amount of hexadecane or hexadecane (g): A- -alkane or mid-alkane arithmetic mean value (A4.7 FPD performance verification
4.7.1 Verification conditions see Table 2.
4.7.2 Base or taste sound and baseline drift verification. According to the verification conditions in Table 2, the measurement method is the same as in 4.6.2. 4.7.3 Detection limit verification
According to the specified conditions in Table 2, put the instrument in the most stable state, wait for the base level to stabilize, and inject the solution with the injection nozzle. A solution of methyl sulfide-free ethanol with a concentration of [0 m] was injected for 1 l-2 l, and the sample was injected 6 times in a row. The peak area of the peak of phosphorus was recorded at the output limit of 12:1 ... Sample scale ();
Peak quotient [mV]:
Peak cage at 1A of the system (
The peak of the preceding atom in the molecule is the base pair of the sparse Coulomb base
The base pair of the sparse Coulomb base
The base pair mass of the sparse Coulomb base
26.124.118
4.BECD Performance range
4.8.1 Test conditions 52
4.B.2 Line media 11 and baseline drift specifications
According to the test conditions in Table 2, select the frequency sensitivity gear, adjust the output signal to record the graph or only display a small part of the graph, after the compensation, record the average value for 2 hours. Calculate the baseline drift and baseline source shift, 4.8.1 Detection limit test
According to the test conditions in Table 2, make the receptor at the maximum temperature, after the temperature and the line are stable, use a microinjection to inject 30.1 package of internal 666-external calcined solution, inject 1~2u, and inject 6 times continuously, record as the internal 666 peak. 4.8.4 Detection limit calculation
Wu Zhong: Pw\
C Detection limit (:
H Line noise (nV):
C Sample injection temperature ():
A Arithmetic compensation of the peak value of 666 (mVrin):
4.9 MFLI performance test
4.9.1 Control conditions see Table 2
4,9.2 Line noise and source effect
According to the conditions in Table 2, select the type and appropriate attenuation, wait for the baseline to stabilize, and record the new line. Measure and calculate the baseline media mountain and line drift,
4.9.3 Detection limit test
Table? Verification conditions: Select a suitable test chamber, use the most accurate camera to inject 10m5/L of isooctylphosphine-isooctanoate at 12°C for 6 times, calculate the arithmetic mean of the peak areas of isooctylphosphine (or isooctylphosphine), 4.9.4 Calculation of the total molar mass of nitrogen contained in the injected sample (w/w): 1-10 atoms of nitrogen, the arithmetic mean value is: w/w = 2 × 14 = 0.154 atoms of nitrogen, or w/w = 2 × 14 = 0.154 atoms of nitrogen. The peak area of the wine is the same as the value of the final product:
and the night energy is the same as the original 331
the correct quality of the wine
4.10 Quantitative reproducibility test
The relative standard deviation R of the peak area measurement is expressed as follows: a
Relative standard deviation (%):
Number of measurements:
The area measured for the first time;
Work——the peak area of n injections is calculated as the average value; i Sample number.
5 Verification result processing and verification cycle
×100%
5.1 Verify the products that do not meet the technical indicators in Table 1 according to the requirements of this procedure. A calibration certificate shall be issued to qualified instruments, and a calibration report shall be issued to unqualified instruments. 5.2 The calibration period of gas chromatograph is 2 years. Appendix A Calibration of microinjection device The microinjection device has good airtightness and should be cleaned and dried before calibration. The water used for calibration should be clean. Calibration method: At room temperature, draw a certain volume of water and cover the needle with a silicone rubber pad. Weigh it on an analytical balance of ten-thousandths of a gram. Then draw out the mercury and weigh it again. The mass of mercury can be obtained by subtraction, and then the actual volume (ml) is calculated according to the following formula: Formula A: V M——The mass of the first weighing (); |The mass of the second weighing (g);
The density of mercury at room temperature (n:l
Each volume point is calibrated 6 times and the arithmetic half mean is taken. The relative standard deviation is within 1%. Appendix H Correction of the rectified gas flow rate
The gas flow rate measured at the detector outlet is corrected by the following formula F,-iF.
Corrected carrier gas flow rate (nl/mun):
Carrier gas flow rate out of the detector measured by soap film flowmeter at room temperature (called): Temperature (K):
Wetness (K:
Saturated vapor pressure of water at room temperature (MPa): Atmospheric pressure (Ma):
Pressure correction factor.
×(p.- po)*
(p pu -
Formula: Note: Base strength (Ma):
Verification certificate and verification result notice] Format Appendix
Verification result
Detector name
Flow rate stability
Box temperature stability
Program temperature rise stress
Base noise
Line displacement
Test instrument replacement error
Appendix: Verification record of gas analyzer
Light unit
Submit to control monoclonal antibody
Money department
After the hair is in place
Night instrument number
Received R period
1 .External measurement:
2.Carrier gas liquid speed qualitative: (m/in)
3.Detection end name:
2.Verification conditions:
Color low +1
Production space repair
Remember tea drop sensitivity seat
Second class
5.Wet stability in the box:
6.Program temperature rise single complex:
7, some money throat sound
8.Line depth shift:
9, Grade high peak surface class:
10.Replacement of reducer to eliminate recognition error:
11.Color latent map number:
12, Preparation:
Brush manufacturing!
Atmospheric F
Test product
Detector pressure
Standard item standard
Single mean value
27 (%)2. Use gas standard for sensitive quality determination. According to the test conditions in Table 2, introduce 10 μmol/wl CH/N standard gas, sample 6 times continuously, and record the peak area of hexadecane. Calculation of detection limit: Tm/FI1) Detection limit (g): N-baseline peak (A); Injection amount of hexadecane or hexadecane (g): A- -alkane or mid-alkane arithmetic mean value (A4.7 FPD performance verification
4.7.1 Verification conditions see Table 2.
4.7.2 Base or taste sound and baseline drift verification. According to the verification conditions in Table 2, the measurement method is the same as in 4.6.2. 4.7.3 Detection limit verification
According to the specified conditions in Table 2, put the instrument in the most stable state, wait for the base level to stabilize, and inject the solution with the injection nozzle. A solution of methyl sulfide-free ethanol with a concentration of [0 m] was injected for 1 l-2 l, and the sample was injected 6 times in a row. The peak area of the peak of phosphorus was recorded at the output limit of 12:1 ... Sample scale ();
Peak quotient [mV]:
Peak cage at 1A of the system (
The peak of the preceding atom in the molecule is the base pair of the sparse Coulomb base
The base pair of the sparse Coulomb base
The base pair mass of the sparse Coulomb base
26.124.118
4.BECD Performance range
4.8.1 Test conditions 52
4.B.2 Line media 11 and baseline drift specifications
According to the test conditions in Table 2, select the frequency sensitivity gear, adjust the output signal to record the graph or only display a small part of the graph, after the compensation, record the average value for 2 hours. Calculate the baseline drift and baseline source shift, 4.8.1 Detection limit test
According to the test conditions in Table 2, make the receptor at the maximum temperature, after the temperature and the line are stable, use a microinjection to inject 30.1 package of internal 666-external calcined solution, inject 1~2u, and inject 6 times continuously, record as the internal 666 peak. 4.8.4 Detection limit calculation
Wu Zhong: Pw\
C Detection limit (:
H Line noise (nV):
C Sample injection temperature ():
A Arithmetic compensation of the peak value of 666 (mVrin):
4.9 MFLI performance test
4.9.1 Control conditions see Table 2
4,9.2 Line noise and source effect
According to the conditions in Table 2, select the type and appropriate attenuation, wait for the baseline to stabilize, and record the new line. Measure and calculate the baseline media mountain and line drift,
4.9.3 Detection limit test
Table? Verification conditions: Select a suitable test chamber, use the most accurate camera to inject 10m5/L of isooctylphosphine-isooctanoate at 12°C for 6 times, calculate the arithmetic mean of the peak areas of isooctylphosphine (or isooctylphosphine), 4.9.4 Calculation of the total molar mass of nitrogen contained in the injected sample (w/w): 1-10 atoms of nitrogen, the arithmetic mean value is: w/w = 2 × 14 = 0.154 atoms of nitrogen, or w/w = 2 × 14 = 0.154 atoms of nitrogen. The peak area of the wine is the same as the value of the final product:
and the night energy is the same as the original 331
the correct quality of the wine
4.10 Quantitative reproducibility test
The relative standard deviation R of the peak area measurement is expressed as follows: a
Relative standard deviation (%):
Number of measurements:
The area measured for the first time;
Work——the peak area of n injections is calculated as the average value; i Sample number.
5 Verification result processing and verification cycle
×100%
5.1 Verify the products that do not meet the technical indicators in Table 1 according to the requirements of this procedure. A calibration certificate shall be issued to qualified instruments, and a calibration report shall be issued to unqualified instruments. 5.2 The calibration period of gas chromatograph is 2 years. Appendix A Calibration of microinjection device The microinjection device has good airtightness and should be cleaned and dried before calibration. The water used for calibration should be clean. Calibration method: At room temperature, draw a certain volume of water and cover the needle with a silicone rubber pad. Weigh it on an analytical balance of ten-thousandths of a gram. Then draw out the mercury and weigh it again. The mass of mercury can be obtained by subtraction, and then the actual volume (ml) is calculated according to the following formula: Formula A: V M——The mass of the first weighing (); |The mass of the second weighing (g);
The density of mercury at room temperature (n:l
Each volume point is calibrated 6 times and the arithmetic half mean is taken. The relative standard deviation is within 1%. Appendix H Correction of the rectified gas flow rate
The gas flow rate measured at the detector outlet is corrected by the following formula F,-iF.
Corrected carrier gas flow rate (nl/mun):
Carrier gas flow rate out of the detector measured by soap film flowmeter at room temperature (called): Temperature (K):
Wetness (K:
Saturated vapor pressure of water at room temperature (MPa): Atmospheric pressure (Ma):
Pressure correction factor.
×(p.- po)*
(p pu -
Formula: Note: Base strength (Ma):
Verification certificate and verification result notice] Format Appendix
Verification result
Detector name
Flow rate stability
Box temperature stability
Program temperature rise stress
Base noise
Line displacement
Test instrument replacement error
Appendix: Verification record of gas analyzer
Light unit
Submit to control monoclonal antibody
Money department
After the hair is in place
Night instrument number
Received R period
1 .External measurement:
2.Carrier gas liquid speed qualitative: (m/in)
3.Detection end name:
2.Verification conditions:
Color low +1
Production space repair
Remember tea drop sensitivity seat
Second class
5.Wet stability in the box:
6.Program temperature rise single complex:
7, some money throat sound
8.Line depth shift:
9, Grade high peak surface class:
10.Replacement of reducer to eliminate recognition error:
11.Color latent map number:
12, Preparation:
Brush manufacturing!
Atmospheric F
Test product
Detector pressure
Standard item standard
Single mean value
27 (%)2. Set the baseline drift and baseline according to the calibration system in Table 2, select the frequency sensitivity level, adjust the output signal to record the graph or only display a small part of the graph, after the compensation, record the average time. Calculate the baseline drift and baseline source drift, 4.8.1 Detection limit calibration According to the calibration conditions in Table 2, make the receptor at the highest level, and after the line is stable, inject the 30.1 package of internal 666-external rate solution with a microinjection, inject 1~2u, and inject 6 times continuously, and record it as the peak value of the 666. 4.8.4 Calculation of detection limit Wu Zhong: Pw\| |tt||C detection limit (：
H line noise (nV):
C sample injection rate ():
A-endosomal 666 peak machine arithmetic compensation (mVrin):
4.9MFLI performance test piece
4.9.1 Control conditions see Table 2
4.9.2 Line noise and source effect
Table 2 4.9.3 Detection limit verification table? Verification conditions: Select a suitable process, use the most accurate camera to inject 12 degrees of 10m5/m-10/m of malathione-isosuccinate, enter the pen 6 times in a row, and calculate the baseline drift. 4.9.4 Calculation of the total molar mass of nitrogen contained in the sample (w/w = 14 × 14 = 0.154) or: w/w = 14 × 14 = 0.154 molar mass of nitrogen contained in the sample The content of 182.2.3
Malathione in the product is the same as the peak area of 331
Malathione. The relative standard deviation R of the peak area measured is calculated according to the following formula: a
t||Relative standard deviation (%):
Number of measurements:
Nth: the area of the peak measured;
Nth: the peak area of the peak injected; i: the sample number.
5 Verification result processing and verification cycle
×100%
5.1 According to the requirements of this regulation, the instrument that does not meet the technical indicators in Table 1 shall be issued a verification certificate, and the unqualified instrument shall be issued a verification certificate. The instrument shall be issued with a certificate of verification. 5.2 The calibration period of gas chromatograph is 2 years. Appendix A Calibration of microinjection device The microinjection device should have good airtightness and should be cleaned and dried before calibration. The water used for calibration should be clean. Calibration method: At room temperature, draw a certain volume of water and cover the needle with a silicone rubber pad. Weigh it on an analytical balance of 10,000th of a gram. Then draw out the mercury and weigh it again. The mass of mercury can be obtained by subtraction, and then the actual volume (ml) is calculated according to the following formula: Formula A: V M——the mass of the first weighing (g); the mass of the second weighing (g); the density of mercury at room temperature (m/s). Calibrate 6 times for each volume point and take the arithmetic half-mean. The relative standard deviation is within 1%. Appendix H Correction of the rectified gas flow rate
The gas flow rate measured at the detector outlet is corrected by the following formula F,-iF.
Corrected carrier gas flow rate (nl/mun):
Carrier gas flow rate at the detector outlet measured by a soap film flowmeter at room temperature (millimeter): Temperature (K):
Humidity (K):
Saturated vapor pressure of water at room temperature (MPa): Atmospheric pressure (Ma):
Pressure correction factor.
×(p.-po)*
(p pu -
Formula: Note: Base strength (Ma):
Verification certificate and verification result notice] Format Appendix
Verification result
Detector name
Flow rate stability
Temperature stability of the test chamber
Program temperature rise stability
Base noise
Linear displacement
Test instrument error
Appendix: Verification record of gas analyzer
Light unit
Submit to control unit
Money contact person
After the contact is completed
Device number
Received period
1. External measurement:
2. Carrier gas liquid velocity qualitative: (m/in)||t t||3. Detection terminal name:
2. Verification conditions:
color low +1
production space repair
remember tea drop sensitivity
secondary grade
5. Humidity stability:
6. Program temperature rise single folding:
7, some money throat sound
8. Line depth shift:
9, high grade peak surface class:
10. Replace the reducer to eliminate the difference:
11. Color potential chart number:
12, equipment:
brush manufacturing!
Atmospheric F
will teach the product
detector pressure
standard item standard
single mean value
27 (%)2. Set the baseline drift and baseline according to the calibration system in Table 2, select the frequency sensitivity level, adjust the output signal to record the graph or only display a small part of the graph, after the compensation, record the average time. Calculate the baseline drift and baseline source drift, 4.8.1 Detection limit calibration According to the calibration conditions in Table 2, make the receptor at the highest level, and after the line is stable, inject the 30.1 package of internal 666-external rate solution with a microinjection, inject 1~2u, and inject 6 times continuously, and record it as the peak value of the 666. 4.8.4 Calculation of detection limit Wu Zhong: Pw\| |tt||C detection limit (：
H line noise (nV):
C sample injection rate ():
A-endosomal 666 peak machine arithmetic compensation (mVrin):
4.9MFLI performance test piece
4.9.1 Control conditions see Table 2
4.9.2 Line noise and source effect
Table 2 4.9.3 Detection limit verification table? Verification conditions: Select a suitable process, use the most accurate camera to inject 12 degrees of 10m5/m-10/m of malathione-isosuccinate, enter the pen 6 times in a row, and calculate the baseline drift. 4.9.4 Calculation of the total molar mass of nitrogen contained in the sample (w/w = 14 × 14 = 0.154) or: w/w = 14 × 14 = 0.154 molar mass of nitrogen contained in the sample The content of 182.2.3
Malathione in the product is the same as the peak area of 331
Malathione. The relative standard deviation R of the peak area measured is calculated according to the following formula: a
t||Relative standard deviation (%):
Number of measurements:
Nth: the area of the peak measured;
Nth: the peak area of the peak injected; i: the sample number.
5 Verification result processing and verification cycle
×100%
5.1 According to the requirements of this regulation, the instrument that does not meet the technical indicators in Table 1 shall be issued a verification certificate, and the unqualified instrument shall be issued a verification certificate. The instrument shall be issued with a certificate of verification. 5.2 The calibration period of gas chromatograph is 2 years. Appendix A Calibration of microinjection device The microinjection device should have good airtightness and should be cleaned and dried before calibration. The water used for calibration should be clean. Calibration method: At room temperature, draw a certain volume of water and cover the needle with a silicone rubber pad. Weigh it on an analytical balance of 10,000th of a gram. Then draw out the mercury and weigh it again. The mass of mercury can be obtained by subtraction, and then the actual volume (ml) is calculated according to the following formula: Formula A: V M——the mass of the first weighing (g); the mass of the second weighing (g); the density of mercury at room temperature (m/s). Calibrate 6 times for each volume point and take the arithmetic half-mean. The relative standard deviation is within 1%. Appendix H Correction of the rectified gas flow rate
The gas flow rate measured at the detector outlet is corrected by the following formula F,-iF.
Corrected carrier gas flow rate (nl/mun):
Carrier gas flow rate at the detector outlet measured by a soap film flowmeter at room temperature (millimeter): Temperature (K):
Humidity (K):
Saturated vapor pressure of water at room temperature (MPa): Atmospheric pressure (Ma):
Pressure correction factor.
×(p.-po)*
(p pu -
Formula: Note: Base strength (Ma):
Verification certificate and verification result notice] Format Appendix
Verification result
Detector name
Flow rate stability
Temperature stability of the test chamber
Program temperature rise stability
Base noise
Linear displacement
Test instrument error
Appendix: Verification record of gas analyzer
Light unit
Submit to control unit
Money contact person
After the contact is completed
Device number
Received period
1. External measurement:
2. Carrier gas liquid velocity qualitative: (m/in)||t t||3. Detection terminal name:
2. Verification conditions:
color low +1
production space repair
remember tea drop sensitivity
secondary grade
5. Humidity stability:
6. Program temperature rise single folding:
7, some money throat sound
8. Line depth shift:
9, high grade peak surface class:
10. Replace the reducer to eliminate the difference:
11. Color potential chart number:
12, equipment:
brush manufacturing!
Atmospheric F
will teach the product
detector pressure
standard item standard
single mean value
27 (%)2 The calibration period of gas chromatograph is 2 years. Appendix A Calibration of microinjection device
The microinjection device has good airtightness and should be cleaned and dried before calibration. The water used for calibration is clean. Calibration method: At room temperature, draw a certain volume of water and cover the needle with a silicone rubber pad. Weigh it on a ten-thousandth gram analytical balance. Then draw out the mercury and weigh it again. The mass of mercury can be obtained by subtraction, and then the actual volume (ml) is calculated according to the following formula:
Formula A: V||tt| ... Correction of the rectified gas flow rate
The gas flow rate measured at the detector outlet is corrected by the following formula F,-iF.
Corrected carrier gas flow rate (nl/mun):
Carrier gas flow rate at the detector outlet measured by a soap film flowmeter at room temperature (millimeter): Temperature (K):
Wetness (K):
Saturated vapor pressure of water at room temperature (MPa): Atmospheric pressure (Ma):
Pressure correction factor.
×(p.- po)*
(p pu -
Formula: Note: Base strength (Ma):
Verification certificate and verification result notice] Format Appendix
Verification result
Detector name
Flow rate stability
Temperature stability of the test chamber
Program temperature rise stability
Base noise
Linear displacement
Test instrument error
Appendix: Verification record of gas analyzer
Light unit
Submit to control unit
Money contact person
After the contact is completed
Device number
Received period
1. External measurement:
2. Carrier gas liquid velocity qualitative: (m/in)||t t||3. Detection terminal name:
2. Verification conditions:
color low +1www.bzxz.net
production space repair
remember tea drop sensitivity
secondary grade
5. Humidity stability:
6. Program temperature rise single folding:
7, some money throat sound
8. Line depth shift:
9, high grade peak surface class:
10. Replace the reducer to eliminate the difference:
11. Color potential chart number:
12, equipment:
brush manufacturing!
Atmospheric F
will teach the product
detector pressure
standard item standard
single mean value
27 (%)2 The calibration period of gas chromatograph is 2 years. Appendix A Calibration of microinjection device
The microinjection device has good airtightness and should be cleaned and dried before calibration. The water used for calibration is clean. Calibration method: At room temperature, draw a certain volume of water and cover the needle with a silicone rubber pad. Weigh it on a ten-thousandth gram analytical balance. Then draw out the mercury and weigh it again. The mass of mercury can be obtained by subtraction, and then the actual volume (ml) is calculated according to the following formula:
Formula A: V||tt| ... Correction of the rectified gas flow rate
The gas flow rate measured at the detector outlet is corrected by the following formula F,-iF.
Corrected carrier gas flow rate (nl/mun):
Carrier gas flow rate at the detector outlet measured by a soap film flowmeter at room temperature (millimeter): Temperature (K):
Wetness (K):
Saturated vapor pressure of water at room temperature (MPa): Atmospheric pressure (Ma):
Pressure correction factor.
×(p.- po)*
(p pu -
Formula: Note: Base strength (Ma):
Verification certificate and verification result notice] Format Appendix
Verification result
Detector name
Flow rate stability
Temperature stability of the test chamber
Program temperature rise stability
Base noise
Linear displacement
Test instrument error
Appendix: Verification record of gas analyzer
Light unit
Submit to control unit
Money contact person
After the contact is completed
Device number
Received period
1. External measurement:
2. Carrier gas liquid velocity qualitative: (m/in)||t t||3. Detection terminal name:
2. Verification conditions:
color low +1
production space repair
remember tea drop sensitivity
secondary grade
5. Humidity stability:
6. Program temperature rise single folding:
7, some money throat sound
8. Line depth shift:
9, high grade peak surface class:
10. Replace the reducer to eliminate the difference:
11. Color potential chart number:
12, equipment:
brush manufacturing!
Atmospheric F
will teach the product
detector pressure
standard item standard
single mean value
27 (%)
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