This specification is applicable to the calibration of ion trap and quadrupole benchtop gas chromatograph-mass spectrometer (hereinafter referred to as benchtop GC-MS). The calibration of other types of benchtop GC-MS can refer to this specification. JJF 1164-2006 Calibration specification for benchtop gas chromatograph-mass spectrometer JJF1164-2006 Standard download decompression password: www.bzxz.net
This specification is applicable to the calibration of ion trap and quadrupole benchtop gas chromatograph-mass spectrometer. The calibration of other types of benchtop GC-MS can refer to this specification.

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National Metrology Technical Specification of the People's Republic of China JJF1164-2006
Calibration Specification for Bench Top GasChromatography-Mass Spectrometers2006-12-08 Issued
2007-03-08 Implementation
The General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China issued JJE1164-2006
Calibration Specification for Bench Top GasChromatography-Mass Spectrometers
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This specification was approved by the General Administration of Quality Supervision, Inspection and Quarantine on December 8, 2006 and will be implemented on March 8, 2007.
Responsible unit: National Technical Committee for Physical and Chemical Metrology Drafting unit: China National Institute of Metrology This specification is interpreted by the National Technical Committee for Physical and Chemical Metrology Main drafters of this specification:
Shao Mingwu
Chen Dazhou
Participating drafters:
Xu Ruifeng
JJF1164—2006
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(China Institute of Metrology)
(China Institute of Metrology)
(China Institute of Metrology)
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Zhongyi Jinzhongcaodian
Scope·
References·
Terms and measurement units
Metrological characteristics·||tt ||Calibration conditions·
Laboratory environment·
Standard materials and reagents·
Calibration equipment
Calibration items and calibration methods··
Appearance inspection·
Resolution
Mass range·
Signal-to-noise ratio:
Mass accuracy·
Measurement repeatability
Gas chromatograph oven temperature control
Library search
Calibration result processing
Recalibration time interval
Appendix A
Calibration record format (for reference)
Appendix B Calibration certificate Format (for reference)
Appendix ℃
Appendix D
Appendix E
Appendix F
Gas chromatography and mass spectrometry parameters
Uncertainty evaluation
JJF1164—2006
Theoretical value of the main ion peak of methyl stearate
Main ion peak of perfluoromonobutylamine
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quE-ei-aC-eC-ae-Coraac-CEC-Nca-iiiKANiKAgaCalibration specification for benchtop gas chromatograph-mass spectrometer This specification is applicable to the calibration of ion trap and quadrupole benchtop gas chromatograph-mass spectrometer (hereinafter referred to as benchtop GC-MS). The calibration of other types of benchtop GC-MS can refer to this specification. Cited documents
JJF1001-1998 "General metrological terms and definitions" JJF1059-1999 "Evaluation and expression of uncertainty in measurement" GB/T15481-2000 "General requirements for the competence of testing and calibration laboratories" GB/T6041-2002 "General rules for mass spectrometry analysis methods" JG (Education Committee) 003-1996 "Verification procedure for organic mass spectrometers" JJG700-1999 "Verification procedure for gas chromatographs" OIML/TC16/SC2/R83 Gas chromatograph/mass spectrometer system for analysis of organic pollutants in water
When using this specification, attention should be paid to using the currently valid versions of the above-mentioned cited documents. 3 Terms and units of measurement
3.1 Resolution
The ability to distinguish two adjacent mass spectrometry peaks. For desktop GC-MS, it is expressed as the peak width at 50% of the peak height of a certain ion peak (half-peak width for short), denoted as Wu2, unit ua3.2 Baseline noise The width between the base peak and the peak valley, unit counts. 3.3 Signal-to-noise ratio The ratio of the signal intensity of the sample to be tested to the baseline noise, denoted as S/N. 3.4 Mass chromatogram The mass spectral data obtained by the mass spectrometer automatically and repeatedly scanning within a certain mass range can be reproduced in different forms, with one or more spectra of ion intensity changing with time, called mass chromatogram. 3.5 Mass accuracy The deviation of the instrument's measured value from the theoretical value.
3.6 u (atomic mass unit)
Atomic mass unit.
4 Overview
Gas chromatograph-mass spectrometer is an analytical instrument that couples gas chromatograph and mass spectrometer together through a certain interface. After the sample is separated by gas chromatography, each component enters the mass spectrometer detector in turn, and the components are ionized in the ion source, 1
JJF1164-—2006
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qUE-ei-aC-eC-ae-Ccraac-CEC-Neca-TrKAoNniKAca to produce ions with certain charges and different mass numbers. Different ions have different motion behaviors in electric and/or magnetic fields. Different mass analyzers are used to separate the charged ions according to the mass-to-charge ratio (m) to obtain a mass spectrum arranged in order of mass. By analyzing and processing the mass spectrum, the qualitative and quantitative results of the sample can be obtained. The gas chromatography-mass spectrometer mainly includes the gas chromatography system (generally without detector), ion source, mass analyzer, detector, vacuum system and computer system.
5 Metrological characteristics
The technical indicators of the desktop GC-MS are shown in Table 1. Table 1 Main technical indicators of desktop GC-MS
Technical indicators
Mass range
Mass accuracy·
Resolution (R)*
Signal-to-noise ratio*
Measurement repeatability
Library search
Gas chromatography column box temperature control
Not less than 600u
100pg octafluoro tea, S/N≥10:1 (peak-to-peak value) at m/=272 10.0ng benzophenone, S/N≥10:1 (peak-to-peak value) at m/183 100 octafluoro tea, S/N ≥ 100:1 (peak-to-peak value) at m/272 RSD ≤ 10%
10ng methyl stearate, similarity ≥ 75%
Column box temperature stability (10min) better than 0.5% Program temperature repeatability better than 2% Note: 1 The standard is the item that must be calibrated:
2 When used for qualitative testing, the standard can be omitted. When used for quantitative testing, the standard must be done, but the customer's own working standard solution can be used, and the indicators can also be determined according to the user's requirements; 3 This technical indicator is for reference only and is not used as a basis for qualification judgment. 6 Calibration conditions
6.1 Laboratory environment
6.1.1 There must be no strong mechanical vibration and electromagnetic interference in the instrument room, and flammable, explosive and highly corrosive gases or reagents not related to the experiment must not be stored.
6.1.2 Laboratory temperature: (15~27)℃. 6.1.3Relative humidity: ≤75%.
6.2 Standard substances and reagents
JJF1164—2006
6.2.1 Octafluoronaphthalene-isooctane solution standard substance: 100pg/uL; 6.2.2 Benzophenone-isooctane solution standard substance: 10.0nglL; 6.2.3 Hexachlorobenzene-isooctane solution standard substance: 10.0ng/μL; 6.2.4 Methyl stearate-isooctane test solution: 10.0ng/μL; 6.2.5 Isooctane or n-hexane: liquid chromatography grade or equivalent. 6.3 Calibration equipment
6.3.1 Micro syringe: 10μL;
SNASTHNA
2 Special measuring instrument for gas chromatograph verification
Calibration items and calibration methods
Appearance inspection
The instrument must not have
7.2 Resolution
Instrument stability
Get half-peak width
1 Adjust
2 Can also
Run at night accurately,
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Execute the Autotm command to perform automatic tuning until the tuning is successful and print the tuning report. The sample used is all triamine (FC43); Manual tuning:
The earliest position at which the tuning report can be printed
7.3 Quality
With full resolution
Above 600
7.4 Signal-to-noise
7.4.1 EI source
amine is the tuning sample into
600) mass spectrum peak
After the instrument is tuned,
extract mlz=272 years
where: H272—
Refer to the appendix
Reproduce the mass
Can be measured and calculated according to the tuning result
Half peak width W
Observe whether the mass
pg/μL of long-term tea
conditions appear, inject 100
|1.0uL of isooctane solution,
Spectrum,
SINH
Extract ion (m/2) peak height;
METROLOGY
H-baseline noise
7.4.2 Positive CI source
Refer to the conditions of 7.4.1, inject 1.0μL of 10.0ng/μL benzophenone-isooctane solution, extract ml=183 ions, reproduce the mass chromatogram, and calculate S/N according to formula (1). 7.4.3 Negative CI source
Refer to the conditions of 7.4.1, inject 1.0μL of 100pg/uL octafluorochlorine-isooctane solution, extract m/=272 ions, reproduce the mass chromatogram, and calculate S/N according to formula (1). 7.5 Mass Accuracy
Refer to the conditions in 7.4.1, inject 1.0uL of 10.0ng/l methyl stearate-isooctane solution, record the measured mass numbers of the main ions of methyl stearate such as 74, 143, 199, 255 and 298, and retain the effective value to 3 decimal places. The theoretical value is shown in Appendix E. Calculate the difference between the measured value and the theoretical value according to formula (2) to evaluate the mass accuracy.
AM=MM理
Where: M,——the average value of three measurements of the i-th ion, u; M理——the theoretical value of the i-th ion, u.
1 Take the average mass number obtained by three scans of the highest point and the two points on its left and right as the actual measurement result: 2 Take the one with the largest absolute difference between the actual measurement value and the theoretical value as the evaluation data for mass accuracy. 7.6 Measurement repeatability
Refer to the conditions of 7.4.1, inject 1.0mL of hexachlorobenzene isozyme solution with a mass concentration of 10.0nglL in 7.2, and extract the characteristic ion of hexachlorobenzene m/=284 for six consecutive times, reproduce the mass chromatogram, integrate the area according to the mass chromatographic peak, and calculate RSD according to formula (3): (, -)
Where: RSD-relative standard deviation,%; 6-1
-hexachlorobenzene: first measurement peak area:
-hexachlorobenzene: arithmetic mean of the peak area of ​​6 measurements: measurement serial number.
Note: For CI source, the corresponding test sensitivity standard material can be used for repeatability measurement. 7.7 Gas Chromatography Column Box Temperature Control
7.7.1 Column Box Temperature Stability
Connect the connection line of the platinum resistance thermometer to the digital multimeter (or the special measuring instrument for chromatograph calibration), then fix the probe of the thermometer in the middle of the column box, set the column box temperature to 70℃ and heat it up. After the temperature stabilizes, observe for 10 minutes, record each change, and find the temperature difference corresponding to the maximum and minimum values ​​of the digital multimeter. The ratio of this difference to the arithmetic mean of the temperature measurement within 10 minutes is the temperature stability of the box. 7.7.2 Program Temperature Rise Repeatability
Carry out program temperature rise repeatability calibration according to the calibration conditions and methods of 7.7.1. Select the initial temperature of 50℃ and the final temperature of 200℃. The heating rate is about 10℃/min. After the initial temperature stabilizes, start the program heating, record the data once per minute until the final temperature stabilizes, repeat this experiment 2 to 3 times, find the maximum relative deviation (ruler,) of the corresponding point, the value should be ≥2%, the result is calculated as follows.
mx=tx100%
Where: t——the maximum temperature of the corresponding point, ℃; the minimum temperature of the corresponding point, ℃;
t——the average temperature of the corresponding point, ℃.
7.8 Library search
According to the total ion flow chromatogram of 7.5 mass accuracy test, the mass spectrum of methyl stearate is obtained. After deducting the background, 4
JJF1164-2006
Search for methyl stearate in the library provided by the system. 8
Calibration result processing
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Ei-ac-ca-Craac-cEc-Neca-rrkAoNiiKAcaA calibration certificate shall be issued according to the calibration result. All calibration items and their results shall be reflected in the certificate. The expression of calibration result shall comply with the requirements of JJF1071-2000 technical specification, including title, laboratory name and address, name and address of the calibration unit, calibration date, traceability and validity of the measurement standard used for calibration, calibration environment and other aspects.
Recalibration time interval
The recalibration time interval of the desktop gas chromatograph-mass spectrometer is determined by the user. It is recommended not to exceed 2 years. Calibration should be performed at any time when replacing important parts, repairing or doubting the performance of the instrument. Appendix A
Commissioning Unit
Unit Address
Contact Telephone
Instrument Model
JJF1164--2006
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Calibration Record Format (For Reference) (Review)
Contact person
Calibration date
ESHOHONIHST
Factory number
Atmospheric pressure
Appearance inspection
2 Gas chromatograph temperature control
Avoidance:
Column box temperature pull
Regeneration:
Program upgrade
Quality range
Standard
Scanning range|| tt||Extraction
Mass accuracy
Theoretical value
Measured value
Measurement repeatability
Standard substance
Area 1
Library search
Environmental temperature
Mass concentration
New fruit
Environmental humidity
Ionization mode
Injection volume
Extraction mode
PUBL ISHING
Ionization mode
MIETROLOCY
Injection volume
Mass concentration
Injection volume
Hit order of library search
Injection volume
Injection mode
Injection mode
Library name
Spectrum similarity
Main experimental conditions
Calibrator
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Appendix B
Client
Client address
Address
Name of measuring instrument
Description
Model specification
Mudel/Type
Manufacturer
Serial No
JJF1164—2006
Calibration certificate format (for reference)
Calibration certificate cover format
Calibration certificate
CALIBRATION CERTIFICATE
Certificate No.
Certificate No.
Conelusian/Opinion
Calibration date
Issued date
Recommended recalibration date
Due date
) Calibration word
Appravedby
Inspector
Inspectedby
Calibrator
Calibrated by
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