Verification Regulation of Gas-Sensitive Chromatograph for Measuring Trace Hydrogen
Some standard content:
Verification Regulation of Gas-Sensitive Chronatograph for Measuring Trace Hydrogen 1996-11-19 Issued on 1996-05-01 Issued on 1997-05-01 by the State Administration of Technical Supervision JIG 916—1996 Verification Regulation of Gas-Sensitive Chronatograph for Measuring Trace Hydrogen HydrogenJJG916—1996
This regulation was approved by the State Technical Supervision Bureau on November 19, 1996, and will be implemented from May 1, 1997.
Responsible unit: Shangyou City Technical Supervision Bureauwww.bzxz.net
Drafting unit: National Standard Material Research Center The technical provisions of the regulation shall be interpreted by the drafting unit. The main drafter of this regulation:
Participating drafter:
Jiang Dongle
J.IG 916—1996
(National Research Center for Standard Materials)
(National Research Center for Standard Materials)
[National Research Center for Standard Materials
(Beijing Dongyi Company)
Technical requirements
Test conditions
Test items and methods
Test result processing and test period
Appendix 1
JJG916—1996
Test certificate and test result notification Appendix 2 Verification Record Format of Notification (Back)
JJG916—1996
Verification Procedure for Gas Chromatography Micro Oxygen Determination Instrument This procedure is applicable to the verification of newly manufactured, in-use and repaired gas chromatography micro hydrogen determination instruments (including industrial and medical micro hydrogen determination instruments):
1. Overview
Gas-sensitive chromatography micro hydrogen determination instrument (hereinafter referred to as the instrument) is a chromatographic instrument using an oxidizing gas as a detector, including hydrogen gas chromatography. After separation, hydrogen is carried into the detector by the carrier gas. The response value of the detector is clearly related to the oxygen content in the gas, and quantitative analysis can be performed by profiling. The instrument consists of a gas system, a sampling system, a separation system, a detection system and a recording or display instrument group or group. Technical requirements
1 Technical designation
11 The standard, detection limit and calibration limit of the newly manufactured instrument shall comply with the requirements of its manual. The calibration repeatability, carrier gas flow re-measurement repeatability and instrument error tolerance shall comply with the specifications in Table 1. 1.2 The calibration of the instrument during use and repair shall comply with the technical indicators in Table 1. Table 1 Main technical indicators include: 1.) Short-term calibration items Baseline value Baseline weight Carrier generation Statistical value Reproducibility 4 Detection limit 5 Reduction error Quantitative gravity Line calibration Maximum allowable error (0-10): 10-^ $0.5 mV/30mi! 2
2A×10-6
Recording type
Digital display stand-reading type
(0 ~100) ×10-n
0.5 mV/30 mn
5.0×10-7
12%
+35 a.10-6
1I x 10**1rol/mol
Note: # Jinghuo Company-Guangzhou 2010, with the standard convection left crown display: * In the figure at (20 ~ 100) 10, with the measurement point relative to the fixed display: t** The hydrogen content H) in this embodiment is shown in the groove mnle clothing, 2 loose war garbage introduction instrument installation requirements
2. Calibration environment
2.1. 1 Ambient temperature: 5-35 Note: JJL 916--1996 Relative humidity: not too high. Verification conditions: no strong mechanical magnetic potential, flammable, explosive and volatile gases. 2.2 Installation requirements: The equipment should be safe and reliable. The cables should be connected tightly and well. The integrated pipeline should be made of polyvinyl chloride pipe without seams. Zhongzhen Anjia: power supply mountain, out of the word into the agreement when the device said the book Hui sought, insulation sheet danger: instrument network small dial when the source, power supply rise US Shi Tong position cover, with 500V pen edge house Ming wheat test product source into the load and the outer Kang theory edge in the slide, width not less than 2, 2.1 set of set
and the signal device certification intention use of the certificate after meter determination qualified: table: the degree value is not .01
note judge: 1I, lead meter inspection tube format: or six pass release fixed car take property: safe flow to certificate: rope behavior will be
number of multi-use table: half
4 standard to material
, Ar's 5 same content body standard material (Table 2 Table 2H, points to the selection of
3... generally low check
(0-0) ×10 *
0.5 × 11-
Verification items and verification methods
Region head
(0.-10); ×10-
1.0×10-5
100×10-6
JJG 9161996
3"The instrument shall be marked with the following: instrument name, instrument number, factory date and comprehensive information 3.2 Under the verification operation conditions, check the joints of the gas source and the gas exhaust of the instrument, and there should be no leakage. Ensure good air tightness:
3.3 The calibrated instrument should be able to adjust normally, and all adjustments, safety devices and switches can work normally without detection phenomenon, and the indicator light should not be sensitive:
Carrier gas flow basic measurement hydrogen performance verification
Select the appropriate reading Carrier gas flow rate, wait for a stable flow through the membrane flow meter, continuously measure 6 times, its relative standard is 1..
5 clothes attenuation error calibration
standard detector performance under certain conditions, check and test the attenuator of the detection machine is no difference, after the instrument is stable, the output end of the instrument is connected to the multimeter, the desired attenuation is ", measure the lower value, the attenuation needs to be placed in the high city, measure in turn until the corresponding value: the attenuator temperature difference should be less than 2 parts: according to () formula: the attenuation error: 4, - kRe Attenuation difference, %: R,—-response value when attenuation is 1/, V, Table 1. Attenuation interval number Ra—response value to skin when attenuation is 1, V, 6.1.1 Spectral separation size: 13× sieve or 5A sieve, inner diameter 2.-3, length 1-2m, 6.1.2 Carrier gas: (1) The industry uses high-purity oxygen. After purification, the hydrogen content is not more than 5.0×10-B, and the carrier gas flow rate is f--20mL/mir: () Medical The model uses air (with a drag air pump) after pure flower, hydrogen content of the hood is 1.0×10, the carrier gas flow is 2030mL/min6.1.3 The thermal current and the upper working voltage are adjusted to the maximum value. 6.2 Set the attenuator to the maximum value, adjust it with the position regulator, and then output the number at the recorded position. After the benzene line is stable, record the basic system 3lm.n, measure the basic system and calculate the basic system. The baseline drift is the detection limit of the gold standard
. 6.1 The instrument is operated on the remaining parts, the gas is introduced into the instrument or the standard attenuator. The gas fraction is 2×10-1. The standard material is 1, and the actual selection is detailed. The relative standard error should be less than % (calculated in the formula of the research formula "2")
! In the free station time limit, the three-way air as the guard of the company: the detection limit of H3 gas is calculated according to formula (2):
In the formula: - detection limit (×10)
N - benzene line noise (mV):
JJG9161996
-2N:3(A:)
- H, component response value obtained under the weighted instrument (mV) - gas standard material H, component mole fraction (×1\); - instrument attenuation effect
8 fixed base repeatability test
Under the working conditions of 6.1, the H component response value [Dong height: mm) is measured 6 times, and the relative standard error (expressed as daily value) is used. Calculate according to formula (3): (R.-R)
Where: v is the symmetrical standard deviation (%):
is the number of measurements;
R is the peak height of the first measurement;
is the arithmetic mean of the peak heights measured for the first time;
is the arithmetic mean of the peak heights measured for the second time;
is the linear standard
Under the instrument working conditions in Article 6.1, according to the measurement range of the H2O component in the same measurement range, select 5 gas standards with different H2O content (see Table 2), measure the response values of the H2O components at the corresponding points in turn, measure each point three times, take the average value, and make a standard curve of the component content against the instrument response value: calculate the linear range and correlation coefficient by the least squares method, and the correlation coefficient should be greater than 0.99. The corresponding component content range is:
The response value corresponding to the lower limit of the standard curve oxygen component content point is not less than 1.2V10 Verification of the maximum allowable error of medical digital direct reading micro oxygen meter 10.1 Maximum allowable error
10.1.1 In the measurement range of less than 20×106, inject 1m with a gas standard substance containing 5×10-6 hydrogen, repeat the measurement 6 times, take the average value, and the maximum allowable error shall not exceed 1×10.6 10.1.2 In the measurement range of less than 20-100×10, inject 1m with a gas standard substance containing 5×10-5 hydrogen, repeat the measurement 6 times, take the average value, and the total relative deviation shall not exceed ±5%. V. Verification result processing and verification period
The qualified instrument shall be issued with the initial verification certificate according to this regulation, and the unqualified instrument shall be issued with the final verification notice, and the fixed period shall be 1 year.
Appendix 1
External soul:
Baseline noise:
Baseline drift:
G 9J6—1996
Verification certificate and verification result notice (on the back) formatVerification result
Carrier gas flow measurement repeatability:
Detection limit:
Setting weight:
Attenuator error:
Linear range:
Indication error:
Appendix 2
Verification plan
Inspection unit
Production manufacturer
Appearance inspection
Carrier gas flow
Q/(nL-min)
Separability
Heating current/nLA
Recorder model
Baseline noise City
Baseline source shift
Name of certified material
Tester
Linear range
H,Response value
Half mean value/()
Core instrument protection band
RUnit
Maximum allowable error
Construction code
Nuclear chastity
JJG:916—1996
Control record format
Factory number
TWorking voltage W
Certificate number
Instrument type
Equipment abbreviation
Average value
Working flow A
Passbook number
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