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GBZT302-2018: Determination of antimony in urine -- Atomic fluorescence spectrometry method
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Determination of antimony in urine -- Atomic fluorescence spectrometry method
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GBZ/T 302-2018
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Basic data | Standard ID | GBZ/T 302-2018 (GBZ/T302-2018) | | Description (Translated English) | Determination of antimony in urine -- Atomic fluorescence spectrometry method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | C60 | | Word Count Estimation | 6,676 | | Date of Issue | 2018-08-16 | | Date of Implementation | 2019-01-01 | | Regulation (derived from) | State-Health-Communication (2018) No.14 | | Issuing agency(ies) | National Health and Family Planning Commission | GBZ/T 302-2018: Determination of antimony in urine -- Atomic fluorescence spectrometry method---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Determination of antimony in urine - Atomic fluorescence spectrometry method
ICS 13.100
C 52
National Occupational Health Standards
Determination of urinary helium in atomic fluorescence spectrometry
Determination of antimony in urine
- atomic fluorescence spectrometry method
Published on.2018 - 08 - 16
2019 - 01 - 01 implementation
National Health and Wellness Committee of the People's Republic of China
Foreword
This standard is formulated in accordance with the Law of the People's Republic
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard is mainly drafted by. School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, Wuhan Occupational Disease Prevention and Treatment Institute, Guangxi Zhuangzu
Administrative District Hospital for Occupational Diseases.
The main drafters of this standard. Zhang Yuzeng, Zheng Dan, Song Weili, Li Rongjuan, Ning Panliang, Huang Zhongke, Chen Weihong, Yan Limei, Jiang Jinfeng,
Chen Zhiliang.
Determination of urinary helium in atomic fluorescence spectrometry
1 Scope
This standard specifies atomic fluorescence spectrometry for the determination of bismuth in urine.
This standard applies to the measurement of urinary fistula in occupational exposure personnel.
2 Normative references
The following documents are indispensable for the application of this document. For dated references, only the dated version applies to this document.
For undated references, the latest edition (including all amendments) applies to this document.
General rules for biological monitoring of GBZ /T 295 occupational population
3 Principle
Urine sample (hereinafter referred to as urine sample) is digested with hydrogen peroxide-nitric acid-nickel nitrate solution, and under acidic conditions, L-cysteine will be five.
The valence is reduced to trivalent ruthenium, and potassium borohydride is added to reduce hydrogen sulfide, which is decomposed into atomic state by argon gas into a quartz atomizer.
The 217.6 nm long hollow cathode lamp emits atomic fluorescence, and the atomic fluorescence intensity is measured. The fluorescence intensity generated is equal to the strontium content in the solution.
Proportional, quantitative compared to the standard curve.
4 instruments
4.1 Packed polyethylene plastic bottle, 100 mL.
4.2 urine hydrometer.
4.3 Erlenmeyer flask, 100 mL.
4.4 Colorimetric tube, 10 mL.
4.5 Pipette, 1.0 mL, 5.0 mL, 10.0 mL.
4.6 Micropipettes, 100 L,.200 L, 1000 L.
4.7 Temperature control electric heating plate.
4.8 Constant temperature water bath.
4.9 Atomic Fluorescence Spectrometer, 锑 Hollow Cathode Lamp.
5 reagent
5.1 The experimental water is deionized water, and the acid is excellent grade.
5.2 Nitric acid, ρ = 1.42 g/cm3.
5.3 Hydrochloric acid, ρ = 1.179 g/cm3.
5.4 Hydrogen peroxide (30%), analytically pure.
5.5 Hydrochloric acid solution. 5% (volume fraction).
5.6 Nickel nitrate solution. 12.5 g/L, take 20 g of nickel nitrate [Ni (NO3) 2 · 6H2O, analytically pure], dissolved in water and diluted to 1000 mL
spare.
5.7 Potassium Hydroxide Solution. 1 g/L, take 0.1 g of potassium hydroxide (excellent grade), dissolve in water and dilute to 100 mL, and prepare before use.
5.8 Potassium borohydride solution. 10 g/L, take 1 g of potassium borohydride (analytical grade), dissolve and dilute to 100 with 1 g/L potassium hydroxide solution
mL, prepared before use.
5.9 L-cysteine solution. 10.0 g/L, take 1 g of L-cysteine (biochemical reagent) in a 100 mL beaker, dissolve in water and dilute
Release to 100 mL, prepared before use.
5.10 锑 standard solution. use the nationally recognized 锑 standard solution.
5.11 Standard application solution. Accurately absorb 2.5 mL of 锑 standard solution (100.0 g/mL) into a 25 mL volumetric flask, and bring up to volume with water.
This is a standard stock solution at a concentration of 10.0 μg/mL. Dilute the standard stock solution to 1.0 μg/mL standard application solution with water.
6 Sample collection, transportation and storage
6.1 According to GBZ /T 295 for urine sample collection, the polyethylene plastic bottle is used to collect the urine sample ≥ 50 mL, and the urine specific gravity is measured in time.
6.2 Sample blank. 2 samples of urine collection with the same batch number as the sample collection were randomly selected as sample blanks.
6.3 Sample transportation. Store the collected samples and sample blanks in a clean container for refrigerated transport.
6.4 Sample storage. It can be stored for 3 days at room temperature, 7 days at 4 °C, and stored for 14 days at -8 °C.
7 Analysis steps
7.1 Instrument operation reference conditions. lamp current is 80 mA, negative high voltage is 270 V, atomizer temperature is.200 ° C, atomizer height is
8 mm, the carrier gas is argon, the carrier gas flow rate is 400 mL/min, the shielding gas flow rate is 800 mL/min, and the measurement method is peak area, current carrying.
5% hydrochloric acid solution, reducing agent. 10 g/L potassium borohydride solution.
7.2 Drawing of the standard curve. Take 6 colorimetric tubes and add 0.0 μL, 20.0 μL, 50.0 μL, 100.0 μL, 150.0 μL, respectively.
200.0 μL of standard application solution, add 0.5 mL of hydrochloric acid, 2.0 mL of L-cysteine solution, and dilute to 10 mL with water.
In the standard series of 0.0 μg/L, 2.0 μg/L, 5.0 μg/L, 10.0 μg/L, 15.0 μg/L, 20.0 μg/L. Reference instrument
Operating conditions, the atomic fluorescence photometer is adjusted to the best measurement state. First enter the blank value measurement state, and continuously use the first tube to obtain the sample.
A stable blank value is obtained, and after the automatic deduction is performed, each standard tube is sequentially determined. The measured fluorescence intensity value and the corresponding erbium concentration (μg/L)
Draw a standard curve (or prepare a standard curve by automating the dilution of the instrument to prepare a standard series).
7.3 Preparation and pretreatment of the sample. Shake the sample thoroughly, take 1.0 mL of urine sample in a conical flask, and add 2 mL of nickel nitrate solution in turn, 3
mL hydrogen peroxide and 5 mL nitric acid, shake well, let stand for 15 min, digest to near dry at 270 °C temperature-controlled electric heating plate, cool to room temperature and then add
Add 0.5 mL of hydrochloric acid, 2 mL of L-cysteine solution, transfer to a 10 mL colorimetric tube, rinse the Erlenmeyer flask with water, and transfer the wash solution into the colorimetric tube.
And make up to 10 mL, 65 ° C water bath for 15 min, mix for measurement.
7.4 Preparation and pretreatment of sample blanks. Sample blanks are prepared according to GBZ /T 173, and samples and samples are added to the urine collection container as a blank.
Collect the equivalent amount of water, take 1.0 mL in the Erlenmeyer flask, and the rest of the processing steps are the same as 7.3.
7.5 Determination of sample and sample blanks. Determine the sample and sample blank solution by measuring the operating conditions of the standard tube. The blank measurement result should be small.
At the limit of detection. When the test result is greater than the detection limit, it indicates that the sample is contaminated during collection, transportation and storage, and the batch sample should be discarded.
The concentration of ruthenium (μg/L) was calculated from the measured fluorescence intensity values using a standard curve.
8 calculation
8.1 Calculate the concentration correction factor (k) in the urine sample converted to the standard specific gravity (1.020) according to formula (1).
1020.1
SG
k (1)
In the formula.
K--converted to the concentration correction factor under the standard specific gravity;
SG-- is the measured specific gravity.
8.2 Calculate the concentration of strontium in urine according to formula (2)
kFCC 0 (2)
In the formula.
C--the concentration of strontium in urine, in micrograms per liter (μg/L);
C0--the concentration obtained from the standard curve in micrograms per liter (μg/L);
F--sample dilution factor;
k--Converted to the concentration correction factor under the standard specific gravity.
9 Description
9.1 The detection limit of the method is 0.06 μg/L, and the lower limit of the method is 0.20 μg/L; the method is 0.20 μg/L to 20.00.
Gg/L (based on 1 mL of urine sample). The relative standard deviation of the precision within the method is 0.51%~3.84%, and the precision between batches is relatively standard deviation.
The difference is 1.55%~4.58%, and the recoveries of standard addition are 98.60%~102.80%. If the sample enthalpy concentration is outside the measurement range, dilute the sample
Determination.
9.2 L-cysteine solution is a metal masking agent and pre-reducing agent to eliminate coexisting ion interference and valence interference. Interference with multiple elements
Experiments revealed that 100 μg/mL of K, Na, Mg2, Zn2, Fe2, Ca2, Mn4, Cu2, Pb2, Hg2; 10 μg/mL
Cr6, Cd2, Se2; 5 μg/mL As3; 1.0 μg/mL Sn2; 0.8 μg/mL Bi2; 12.5 g/L Ni2
There is no interference at all. L-cysteine also eliminates the valence interference of strontium.
9.3 Collect urine samples from the end of the work of the contact person. The urine samples should be taken out of the site environment, replaced with overalls, and washed hands to prevent pollution.
9.4 The glass instruments and plastic hoses used are first soaked in 50% hydrochloric acid solution for 24 h, then soaked in 10% nitric acid solution for 24 h, and finally water
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