GBZ/T 308-2018_English: PDF (GBZ/T308-2018)
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Simultaneous determination of a variety of metals in urine -- Inductively coupled plasma mass spectrometry method
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GBZ/T 308-2018
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Standard ID | GBZ/T 308-2018 (GBZ/T308-2018) | Description (Translated English) | Simultaneous determination of a variety of metals in urine -- Inductively coupled plasma mass spectrometry method | Sector / Industry | National Standard (Recommended) | Classification of Chinese Standard | C60 | Word Count Estimation | 7,783 | Date of Issue | 2018-08-16 | Date of Implementation | 2019-01-01 | Regulation (derived from) | State-Health-Communication (2018) No.14 |
GBZ/T 308-2018
Simultaneous determination of a variety of metals in urine - Inductively coupled plasma mass spectrometry method
ICS 13.100
C 52
National Occupational Health Standards
Simultaneous determination of inductively coupled plasmas in various metals in urine
Mass spectrometry
Simultaneous determination of a variety of metals in urine
Inductively coupled plasma mass 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 was drafted. Guangdong Provincial Occupational Disease Prevention and Treatment Institute, China Center for Disease Control and Prevention, Occupational Health and Poison Control Institute, Jiangsu Province
Disease Prevention and Control Center, Shenzhen Longgang District Center for Disease Control and Prevention, Shenzhen Luohu District Center for Disease Control and Prevention, Qingyuan City Disease Prevention
control center.
Drafters of this standard. Dong Ming, Zhang Aihua, Wu Banghua, Yan Xiaolin, Ding Chunguang, Liu Dezhen, Zhu Alcohol, Ye Min, He Jianfei, Liu Eryan,
Cui Fan, Pan Qiaoyu, Sun Yi, Yang Zhanhong.
Simultaneous determination of various metals in urine by inductively coupled plasma mass spectrometry
1 Scope
This standard specifies inductively coupled plasma mass spectrometry for simultaneous determination of vanadium, chromium, cobalt, cadmium, antimony and lead in urine.
This standard applies to the determination of vanadium, chromium, cobalt, cadmium, antimony and lead in the urine of occupational contacts.
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.
GBZ /T 295 General rules for occupational health biological monitoring
3 Principle
The urine sample (hereinafter referred to as the urine sample) is diluted with a nitric acid solution and directly injected. Determination of vanadium (V) by inductively coupled plasma mass spectrometry
Concentrations of chromium (Cr), cobalt (Co), cadmium (Cd), thallium (Tl), and lead (Pb).
4 instruments
4.l Inductively coupled plasma mass spectrometer with collision cell.
4.2 Ultrapure water preparation instrument.
4.3 stoppered polyethylene plastic bottle, 100 mL.
4.4 polyethylene plastic tube, 5 mL.
4.5 Micropipettes, 5000 L, 1000 L,.200 L, 50 L.
4.6 Glass instruments and plastic utensils should be soaked in 20% nitric acid for more than 24 hours, rinsed, and dried for use.
5 reagent
5.1 Experimental water. deionized water or double distilled water.
5.2 Nitric acid (HNO3), ρ20=1.42 g/mL, excellent grade pure or high purity.
5.3 Nitric acid solution, 1% (volume fraction). Measure 1.0 mL of HNO3 and add to 99.0 mL of deionized water.
5.4 standard solution. vanadium, chromium, cobalt, cadmium, antimony, lead single element standard solution or mixed standard solution.
5.5 Internal standard solution. It is recommended to use 钇 (Y), indium (In), 钬 (Ho) single element standard solution or mixed standard solution.
5.6 Tuning solution. Lithium (Li), yttrium (Y), cerium (Ce), cerium (Tl), cobalt (Co) single element standard solution or mixing is recommended.
standard solution.
5.7 Standard stock solution and standard application liquid. Mix standard solution of vanadium, chromium, cobalt, cadmium, antimony and lead with nitric acid solution to make 10.0 g/mL mixture
Standard stock solution, diluted with standard nitric acid solution to 1.0 g/mL mixed standard application solution.
5.8 Internal standard stock solution and application liquid. The standard solution of bismuth, indium and bismuth is prepared into a concentration of 10.0 g/mL internal standard stock solution with nitric acid solution.
The internal standard stock solution was diluted to 10.0 g/L of the internal standard application solution with a nitric acid solution.
5.9 Tuning stock solution and application liquid. Prepare a standard solution of lithium, strontium, barium, strontium and cobalt with a nitric acid solution to a concentration of 10.0 g/mL.
Dilute to 10.0 g/L of the tuning solution with a nitric acid solution at the time of use.
6 Sample collection, transportation and storage
Collect urine samples according to GBZ /T 295, collect polyethylene samples from contact or poisoned patients with polyethylene plastic bottles, mix well, and do
Quickly measure urine creatinine or specific gravity, add 1 mL of nitric acid to 100 mL of urine sample, transport as soon as possible at room temperature, and save at least 2 °C~6 °C
14 d.
7 Analysis steps
7.1 Instrument Operation Reference Conditions
RF power 1450 W; cooling gas flow 15 L/min, carrier gas flow 0.85 L/min, auxiliary gas flow 0.25 L/min; scanning mode.
Full quantification; integration time 0.1 s; acquisition times 3 times; cobalt, cadmium, antimony and lead were measured in standard mode. reaction cell inlet voltage -30 V,
The cell outlet voltage is -28 V, the quadrupole lens is at -3 V, and the octopole deflection voltage is -6 V. Vanadium and chromium are measured in collision mode.
The cell inlet voltage is -40 V, the cell outlet voltage is -38 V, the quadrupole focus lens voltage is -13 V, and the octopole deflection voltage is -16 V. Push
It is recommended to use bismuth, indium and antimony as the internal standard elements of the element to be tested, as shown in Table 1. The method of introducing internal standard on-line is used for the determination.
Table 1 Recommended mass and internal standard elements of the element to be tested
The mass of the element to be tested, the mass of the internal standard element
Vanadium (V) 51 钇 (Y) 89
Chromium (Cr) 53 钇 (Y) 89
Cobalt (Co) 59 钇 (Y) 89
Cadmium (Cd) 111 Indium (In) 115
铊(Tl) 205 钬(Ho) 165
Lead (Pb) 208 钬 (Ho) 165
7.2 Instrument Tuning
The plasma is ignited at the start, and after the instrument is preheated for 30 minutes, the tuning liquid is used for mass correction and resolution verification to make the element contained in the tuning liquid.
Sensitivity, precision, mass axis and peak width meet the requirements of the instrument; at the same time, the oxide interference is less than 1.5%, and the double charge interference is small.
At 3.0%.
7.3 Sample Processing
Shake the urine sample, pipette the urine sample into 0.25 mL polyethylene plastic tube, add 4.75 mL nitric acid solution, mix well, and test;
The urine sample was replaced with 0.25 mL of deionized water and treated as the reagent blank. If the content of metal to be tested in urine exceeds the determination of this method
The range can be determined by increasing the dilution factor.
7.4 Drawing of standard curve
Take 6 100 mL volumetric flasks and dilute the standard application solution with nitric acid solution to prepare a standard curve series with a concentration of 0μg/L~10μg/L.
Referring to the operating conditions of the instrument, the element to be tested and the element of the internal standard are determined, and the ratio of the signal value of the element to be tested to the signal value of the internal standard element is the ordinate.
The concentration of the element to be tested is the abscissa, and a standard curve is drawn.
7.5 Sample determination
The sample and the reagent blank solution are determined by measuring the operating conditions of the standard series, and the measured signal value of the sample is subtracted from the reagent blank signal value.
The concentration of the element to be tested (g/L) is derived from the standard curve.
8 calculation
8.1 Calculate the concentration of the element to be tested in urine according to formula (1).
FCC 0 (1)
In the formula.
C--the concentration of the element to be tested in urine, in micrograms per liter (g/L);
C0--the concentration of the element to be tested as found by the standard curve, in micrograms per liter (g/L);
F - urine sample dilution factor.
8.2 Correct the sample results using creatinine or specific gravity calibration methods according to the limits.
9 Description
9.1 The method determines the measurement range by combining the background value and the biological limit of the element to be tested, and the linear relationship of each element in the measurement range is good, and the method
See Table 2 for the detection limits, lower limit of quantitation, recovery, and precision.
Table 2 Performance indicators of the method
element
name
Element
quality
The detection limit
Gg/L
Quantitative lower limit
Gg/L
Intra-assay precision
Inter-assay precision
Recovery rate
Vanadium V 51 0.36 1.19 0.46~4.46 0.72~5.12 92.5~102.1
Chromium Cr 53 0.57 1.91 0.80~5.72 1.70~7.19 87.3~102.1
Cobalt Co 59 0.09 0.29 0.62~4.72 0.89~6.20 92.3~105.8
Cadmium Cd 111 0.06 0.19 0.99~5.92 0.49~5.68 88.2~94.1
铊Tl 205 0.32 1.08 0.53~5.22 0.50~7.16 86.2~104.5
Lead Pb 208 1.67 5.57 0.68~6.10 0.75~6.07 89.8~109.2
9.2 The internal standard element and internal standard solution concentration in this method are recommended applications. In actual work, the undetected elements in the urine and the elements to be tested can be selected.
Other elements with similar masses are used as internal standard elements, and the concentration of the internal standard solution should match the concentration of the element to be tested;
Introduced online or added directly to the sample.
9.3 The nitric acid used in this method is superior grade pure nitric acid. If the background of the element to be tested is higher in nitric acid, it needs to be used after distillation.
9.4 If there is sediment after the urine sample is placed, it must be shaken and measured. For samples of unknown concentration, the dilution factor should be increased.
9.5 Other common elements in the urine sample do not interfere with the determination.
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