JJG 939-1998 Non-dispersive atomic fluorescence photometer JJG939-1998 standard download decompression password: www.bzxz.net
This procedure is applicable to the verification of single-channel and double-channel non-dispersive atomic fluorescence photometers using hollow cathode lamps as light sources, which are newly manufactured, in use or after repair.

National Metrology Verification Regulations of the People's Republic of China JJG 939 —1998
Non -- disperse Atomic Fluorescence Spectrorneter
Published on July 14, 1998
Implemented on January 15, 1999
Published by the State Administration of Quality and Technical Supervision
Verification Rcgulation of
Non - disperse Atomic
Fluorescence Spectrometer
JJG939
This verification procedure was approved by the State Administration of Quality and Technical Supervision on July 14, 1998, and will be implemented on January 15, 1999.
Responsible unit:
Drafting unit:
National Physical and Chemical Metrology Technical Committee
Hebei Metrology and Testing Institute
The drafting unit is responsible for interpreting the technical text of this procedure. The main drafters of this procedure:
Ren Yanli
Qi Erkuang
Dengjia Drafter:
Ma Jinmiao
JJG 939—1998
(Hebei Institute of Metrology and Testing)
(Hebei Institute of Metrology and Testing)
(Hebei Product Quality Supervision and Inspection Institute) (Hebei Institute of Metrology and Testing)
(Hebei Institute of Metrology and Testing)
Technical requirements
Electronic conditions
Verification items and verification methods
Verification result treatment and verification period
Appendix 1 Verification reagents:
Appendix 2 Verification record format
JJG 939
Appendix 3 Verification certificate and verification result notification (back) format Appendix 4 Linear regression method 1 Drawing curve
Appendix 5 Verification strength hollow negative alarm lamp stability (temporary) test method (1)
JJG 939 ——1998
Verification Procedure for Non-Dispersive Atomic Fluorescence Photometer This procedure is applicable to the verification of single-channel and double-channel non-dispersive hydride ion fluorescence photometers (hereinafter referred to as the instrument) using hollow cathode lamps as light sources, which are newly manufactured, in use and after repair: 1. OverviewbZxz.net
This instrument can be used for elements that are easy to form hydrides, elements that are easy to form gas components and elements that are easy to reduce to atomic vapor.
This instrument uses the characteristic incident light emitted by the light source to irradiate the atomic vapor of the measured element, and the ground state atoms are excited to a high energy level. When they are activated by the radiation and return to the ground state, they emit light to perform dating. The fluorescence intensity and the concentration of the element have the following relationship: Ir = l(-e-hr)
Where: original fluorescence intensity;
——atomic fluorescence quantum efficiency;
「. —Radiation intensity of light source;
-Peak absorption coefficient at wavelength L; L
-Absorption optical path:
W is the number of atoms per unit length.
For a given element, when the wavelength and intensity of the light source are specified, the absorption wavelength is fixed, the atomization conditions are constant, and the element concentration is low, the fluorescence intensity and the mass concentration e of the fluorescent substance have the following simple relationship (in terms of band numbers): fr=ap
The block diagram of the device is shown in Figure 1.
High-intensity hollow electrode lamp
Atomizer-Detection system
Atomizer
II. Technical requirements
1 Appearance and preliminary inspection
I.1 The atomizer should have the following marks: instrument name, model, manufacturer's name, factory number and factory date, manufacturing license mark and number, etc.
1.2 All firmware of the instrument and its accessories should be in good condition, the connecting parts should be well connected, the moving parts should be stable and move freely.
1.3 The switches, knobs and buttons of the instrument should be able to work normally. When the keyboard inputs commands for the instrument controlled by a computer, the corresponding functions should be normal.
The instrument must meet the technical specifications and technical indicators shown in Table 1 in 1998
Table 1 Verification items and technical indicators
Stability
Output limit
Time
Deviation from standard
Time to
Newly manufactured
Note: There are inspection items on the instrument, and the financial standard instrument is measured in the same year, and multiple standards are proposed. 3 Calibration environment conditions
31 The instrument room should be bright, clean, dust-free, light-corrosive gas, and well ventilated: 10%
During use
and after use
3.2 The instrument should be placed on a stable and motionless platform. There should be an exhaust system above the instrument. There should be no strong electric field nearby.
3.3 The ambient temperature should be (15-30)%℃ and relatively stable. The relative humidity should not be greater than: 3.4 The power supply voltage of the instrument is (220122)V, and the frequency is (50±1)Iz. Three calibration conditions
4 Test equipment
4.1 High-intensity hollow cathode lamp: As, Sh, the stability of its ignition performance should meet the requirements of Appendix 5.4.2 Sand meter, graduation value 0.13.
4.3Mgohmmeter: test voltage 500V
4.4A-grade glass reactor: 1mml, 200ml, upper (Kmml) container bottles, 5ml, 10ml, 20ml single-line pipettes
Injector: 1rl, 2ml.
Standard: maximum volume 200g or 500g, graduation value ≤: 0.1g4.6
Testing reagents: see Appendix 1 for details:
IV. Verification items and verification methods
5. Appearance and preliminary inspection
The appearance and preliminary inspection of the instrument should comply with the provisions of the first series: 3
6. Stability
JJGF 939 —1998
machine, ignite arsenic and lamp, adjust the current in the lamp to (30~90) mA, set the negative voltage to about 300V, preheat for 30min, and perform analog recording. The initial value of the light intensity of the analog book number is 2002, and the continuous measurement is 30min. The stability of the instrument (maximum drift divided by the initial value) and transient sound (peak-to-peak divided by the initial value) should meet the requirements of the test limit 1.
In order to check the linearity of the limit value,
7.1 Adjust all parameters of the instrument to the best working state, use sodium hydride (or boron hydride) as the reducing agent (the following items all use this reducing agent), and measure the solution and the arsenic and potassium standard mixed solution spanning two numerical levels in Table 2 for 3 times respectively. After the average range, the correlation coefficient and slope of the curve are obtained by linear regression method. tpxw
Where: p——solution mass change (ml): injection potential product [ml)
7.2 Under the same conditions as in 7.1, measure the fluorescence intensity of the free solution 11 times in succession and calculate its standard deviation s.:
Where: f-
The fluorescence intensity value of a single measurement:
(a7m)
—the arithmetic mean of the fluorescence intensities measured once: number of measurements.
7.3 The following formulas are used to calculate the detection limits of the instrument for As and Sb respectively: Q(x=3)=35/6(ng)
8 Relative standard deviation
In the determination of item 7, the standard mixed solution of As and Sb with concentrations of As10.[mg/ml and Sh1.0rp/ml is measured 7 times continuously (for the instrument in use, A20.0ng/1rl and S20.0ru/ml can be used for measurement), and the injection number is less than 2 times. During the measurement, the lamp current and the negative high voltage fluorescence intensity value are adjusted to 200, and the relative standard deviation is calculated: (RS)
Where: $
×%
7 The relative standard deviation of the measurement is calculated by formula (2): The average value of the 1-7 measurements.
In channel 9, select the antibody (channel A) against the antibody (channel B), using l000/ml and Sb10 in Table 2.0/blood standard mixed economic epidemic is measured, and the arithmetic mean is taken for 3 measurements, that is, the value of the B channel measured by any 4 channels (or lamps) is measured 3 times and the arithmetic mean is taken for the channel: 1, and the above formula is used to calculate the interference between channels. RE-1a-1a 100%
10 Insulation resistance
When the instrument is turned on and not connected, use 5V megawatts to measure the resistance between the phase line of the power plug: the cable shell (instrument J3G 939-1998
instrument grounding wire), which should comply with the provisions of Table 1. 11 Newly manufactured instruments must be fully calibrated in Articles 5 to 10, and instruments in use and after repair should be calibrated in Articles 6 to 9 in principle.
V. Verification result processing and verification cycle
12 For instruments that pass the verification, a verification certificate will be issued: for instruments that fail the verification, a verification result notice will be issued. 13 For dual-channel instruments, if the interference between channels is not qualified and other items are qualified, a calibration certificate can be issued, but it is noted that it should be used as a single-channel instrument.
The calibration period is 1 year. During this period, when the components are changed or the measurement results are in doubt, calibration should be carried out at any time
Appendix 1
Oxygen purity 9.99%,
Hydrochloric acid: high-grade purity.
.I3G 939 --1998
Testing reagents
Sodium hydride (potassium hydroxide): purity not less than 95% 3
Sodium hydroxide (potassium hydroxide): analytical grade. 4
Pulse: analytical grade.
Di-ionized water.
The ambient temperature during the calibration of sodium hydride (potassium hydride) solution, the sample injection method of the instrument, the mass concentration of the required sodium hydride (potassium hydride) solution is between (4.0-20.0) g/L, and the solution with a mass concentration of 7.0e/T is prepared: weigh 7.0g sodium hydride (potassium hydride), add 2.0g sodium hydride (potassium hydride) to about 200ml of water, stir until fully submerged, and then dilute with deionized water to 1(00m, if necessary, filter with absorbent cotton. 8100/T. Preparation of sulfur gland
Weigh 20.0g sulfur gland, drop it into a 200ml volumetric flask, and dilute to the scale with primary deionized water. 9 Monument, antimony Standard storage solution; As1000mg/ml and Sb1000g/ml, A=100ng/ml and Sh100r/ml, Ag10.0ng/ml and Sb10.0ng/ml and Ag100DDng/ml and Sb100g/ml standard mixed solution, 10 calibration solution, standard mixed solution: prepared according to work needs, the prepared standard solution concentration uncertainty is shown in Table 2.
Table 2 Mass concentration and uncertainty of calibration solution, standard mixed solution concentration (ng/ml)
Standard mixed solution concentration (ng/ml)
Ab + Sb
0.00 + 0.00
0.50 + 0.50
5.00 +5.00
10.0+10.0
20.0+20.0
50.0 + 50.0
100+10
Preparation method of mixed antimony and antimony for testing When preparing, take the standard circulating rate solution
The concentration
(ng/ml)
0.00 + 0.00
10.0+10.0
10.0+10.0
100+100
100 +100
100 100
1000+1000
1 00+ 1 000
10 000 + 100
Aa + Sb
Take 100g/1
Yu gland【ml】
Take hydroxyhydrochloric acid
Dilute with water to
Preparation product
Uncertainty
Appendix 2
Factory No.
Inspector
1 Appearance and preliminary inspection:
2 Stability: The lamp has been flowing
When measuring, it should be 30
JJG 939 —1998
Verification record format
Non-dispersive fluorescence light meter verification record format Regularly
Clear!
Equipment number
Original record number
Certificate and approval number
British commercial pressure
Stability
3Represents the detection limit of the system, the linearity of the working line: o (ug/ml)
Pour liquid
(11 times)
Lamp current:
Sensitivity:
Compressive pressure:
Injection volume:
Detection limit;
Correlation coefficient:
4Represents the relative standard deviation of the element
Lamp current:
= ng/ml)
=ng/al)
5 Channel Interference
Reading is the formula
Effective channel reading
Single number
Mixed liquid concentration:
Injection volume:
Insulation resistance
Negative high voltage:
Lamp current:
JJG 939 ——1998
Injection volume:
Negative high voltage:
Relative standard deviation
Inter-channel interference
Appendix 3
Stability
J3G 939
Verification certificate and verification result notice (back) format Verification result
Appearance and cutting step inspection
Instantaneous noise
Detection limit
Relative standard deviation
Correlation coefficient
Interference avoidance
Electrical00 + 0.00
10.0+10.0
10.0+10.0
100+100
100 +100
100 100
1000+1000
1 00+ 1 000
10 000 + 100
Aa + Sb
Take 100g/1
Yu gland【ml】
Take hydroxy hydrochloric acid
and dilute it with water to
preparation volume
Uncertain Appendix 2 Factory No. Inspector 1 Appearance and preliminary inspection: 2 Stability ：The lamp has been flowing
When measuring, 30
JJG 939 —1998
Verification record format
Non-dispersion source fluorescence light width meter verification record format regularly||tt ||Scrape it clean!
Equipment No.
Original Record No.
Certificate and Pass Book No.
British Commercial Pressure
Stability
3 Representatives Detection limit, linearity of working line: o (ug/ml)
Drop liquid
(11 times)
Lamp current:
Sensitivity ：
Compressor pressure:
Injection volume:
Detection limit;
Correlation coefficient:
4 represents the relative standard deviation of the element| |tt||Lamp current:
= ng/ml)
=ng/al)
5 channel interference
reading is formula
effective channel reading
single number|| tt||Mixed liquid concentration:
Injection volume:
Insulation resistance
Negative high voltage:
Lamp current:
JJG 939 ——1998
Injection volume:
Negative high pressure:
Relative standard deviation
Channel-to-channel interference
Appendix 3
Stability|| tt||J3G 939
Verification certificate and verification result notice (back) format Verification result
Appearance and cutting step inspection
Instantaneous noise
Detection limit
Relative Standard deviation
Correlation coefficient
Interference
Baoyuan electric00 + 0.00
10.0+10.0
10.0+10.0
100+100
100 +100
100 100
1000+1000
1 00+ 1 000
10 000 + 100
Aa + Sb
Take 100g/1
Yu gland【ml】
Take hydroxy hydrochloric acid
and dilute it with water to
preparation volume
Uncertain Appendix 2 Factory No. Inspector 1 Appearance and preliminary inspection: 2 Stability ：The lamp has been flowing
When measuring, 30
JJG 939 —1998
Verification record format
Non-dispersion source fluorescence light width meter verification record format regularly||tt ||Scrape it clean!
Equipment No.
Original Record No.
Certificate and Pass Book No.
British Commercial Pressure
Stability
3 Representatives Detection limit, linearity of working line: o (ug/ml)
Drop liquid
(11 times)
Lamp current:
Sensitivity ：
Compressor pressure:
Injection volume:
Detection limit;
Correlation coefficient:
4 represents the relative standard deviation of the element| |tt||Lamp current:
= ng/ml)
=ng/al)
5 channel interference
reading is formula
effective channel reading
single number|| tt||Mixed liquid concentration:
Injection volume:
Insulation resistance
Negative high voltage:
Lamp current:
JJG 939 ——1998
Injection volume:
Negative high pressure:
Relative standard deviation
Channel-to-channel interference
Appendix 3
Stability|| tt||J3G 939
Verification certificate and verification result notice (back) format Verification result
Appearance and cutting step inspection
Instantaneous noise
Detection limit
Relative Standard deviation
Correlation coefficient
Interference
Baoyuan electric
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