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GBZT305-2018: Determination of manganese in urine -- Graphite furnace atomic absorption spectrometry method
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| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| GBZ/T 305-2018 | English | 119 |
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Determination of manganese in urine -- Graphite furnace atomic absorption spectrometry method
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GBZ/T 305-2018
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Basic data | Standard ID | GBZ/T 305-2018 (GBZ/T305-2018) | | Description (Translated English) | Determination of manganese in urine -- Graphite furnace atomic absorption spectrometry method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | C60 | | Word Count Estimation | 6,629 | | 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 305-2018: Determination of manganese in urine -- Graphite furnace atomic absorption spectrometry method
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Determination of manganese in urine - Graphite furnace atomic absorption spectrometry method
ICS 13.100
C 52
National Occupational Health Standards
Determination of manganese in urine - Graphite furnace atomic absorption spectrometry
Determination of manganese in urine -
Graphite furnace atomic absorption spectrometry method
Published on.2018 - 08 - 16
2019 - 01 - 01 implementation
National Health and Wellness Committee of the People's Republic of China
GBZ
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. Shenzhen Occupational Disease Prevention and Control Institute, Guangdong Provincial Occupational Disease Prevention and Control Institute, Shenzhen Luohu District Disease Prevention and Control
Heart, Shenzhen Yantian District Center for Disease Control and Prevention.
The main drafters of this standard. Huang Xianqing, Li Tianyu, Zhang Wen, Yan Jianpei, Zhang Aihua, Dong Ming, Lai Shaoyang, Ye Min, Cao Xiaoyun, Lu
Haiyan.
Determination of manganese in urine - Graphite furnace atomic absorption spectrometry
1 Scope
This standard specifies graphite furnace atomic absorption spectrometry for the determination of manganese in urine.
This standard applies to the determination of manganese 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.
General rules for biological monitoring of GBZ /T 295 occupational population
3 Principle
Urine sample (hereinafter referred to as urine sample) is diluted with 1% nitric acid solution and directly used in graphite furnace atomic absorption spectrometry at a wavelength of 279.5 nm.
The method measures the concentration of manganese in the urine.
4 instruments
4.1 Covered wide-mouth polyethylene plastic bottle. 100 mL.
4.2 urine hydrometer.
4.3 with colorimetric tube. 10 mL.
4.4 vortex oscillator.
4.5 Volumetric flask. 10 mL, 50 mL, 100 mL.
4.6 Scale pipette. 1 mL, 2 mL, 10 mL.
4.7 Atomic Absorption Spectrometer. with graphite furnace, Zeeman or xenon lamp background correction device and manganese hollow cathode lamp.
5 reagent
5.1 Experimental water. deionized water.
5.2 Nitric acid, ρ20=1.42 g/mL, excellent grade pure.
5.3 Nitric acid solution, 1 % (V/V).
5.4 Standard solution, using nationally recognized manganese single element standard solution.
5.5 Quality control sample. standard urine sample, contact person mixed urine or spiked normal person mixed urine.
6 Sample collection, transportation and storage
6.1 Environmental conditions. The place where the urine is collected should be clean and tidy, and there is no source of manganese pollution.
6.2 Sample collection. Collect about 50 mL of urine once in a wide-mouth polyethylene plastic bottle, mix well, and take out part of the urine to measure the specific gravity as soon as possible.
Nitric acid was added in a ratio of 1% by volume. If the urine specific gravity is < 1.010 or >1.030, it should be resampled.
6.3 Sample transport. The collected samples can be transported at room temperature.
6.4 Sample storage. The sample can be stored in the refrigerator at 0 °C ~ 4 °C for 14 days.
7 Analysis steps
7.1 Instrument operating conditions
The atomic absorption spectrometer was adjusted to the optimum measurement state with reference to the instrument conditions of Table 1.
Table 1 Instrument operation reference conditions
Instrument condition
Graphite furnace condition
Step temperature
Warming slope
°C/s
Residence time
Wavelength 279.5 nm Dry 50~110 20 10
Slit 0.2 nm 110～130 5 15
Lamp current 9.6 mA Ashing 1000 150 20
Injection volume 10 μL atomization 1800 0 3 (discontinued)
Carrier gas argon 0.2 L/min cleaning 2500 0 4
Graphite tube pyrolysis coating - - - -
Background correction Zeeman or Xenon lamp - - - -
7.2 Sample Processing
After the collected urine sample is placed at room temperature, mix well, take 2.0 mL in a plug colorimetric tube, add 8.0 mL nitric acid solution, mix
After uniformity, it can be directly measured. Take a nitric acid solution as a reagent blank.
7.3 Preparation and determination of uranium manganese standard series
7.3.1 Dilute the manganese single element standard solution to a 20 μg/L standard application solution with a nitric acid solution. Take 7 10 mL volumetric flasks, numbered
For the 1~7, take the above manganese standard application solution 0.0 mL, 1.0 mL, 2.0 mL, 3.0 mL, 4.0 mL, 5.0 mL, 6.0 mL, respectively.
The nitric acid solution was made up to the mark and formulated into 0 μg/L, 2 μg/L, 4 μg/L, 6 μg/L, 8 μg/L, 10 μg/L, and 12 μg/L manganese standard series.
7.3.2 Refer to the instrument operation reference conditions, adjust the atomic absorption spectrometer to the best measurement state, and measure each standard series, 2~7
After subtracting the absorbance value of No. 1, the absorbance value is plotted against the manganese concentration (μg/L) or the regression equation is calculated.
7.4 Sample determination
The sample and reagent blanks are determined using the operating conditions of the assay standard series, and the absorbance values of the sample tubes are subtracted from the absorbance values of the reagent blanks.
The concentration of manganese (μg/L) is then calculated from a standard curve or a regression equation.
8 calculation
Calculate the concentration of manganese in the urine according to formula (1).
000.1
000.1020.1
FCX ...(1)
In the formula.
X--the concentration of manganese in urine, in micrograms per liter (μg/L);
C--the concentration of manganese in the diluted urine sample obtained from the standard curve, in micrograms per liter (μg/L);
F--dilution factor;
G--The specific gravity of the urine sample.
9 Description
9.1 The detection limit of this method is 1.5 μg/L, and the lower limit of quantification is 5.0 μg/L (according to 2.0 mL urine sample, 5 times dilution), the measurement range is
5.0 μg/L to 60 μg/L (in terms of urine). The relative standard deviation range is RSD=1.1%~7.0% (urinary manganese concentration 13.3 μg/L～51.5
Gg/L, n = 6); urine sample spike recovery range of 84.1% ~ 105.8 % (spiked concentration of 10μg/L ~ 40 μg/L).
9.2 About the instrument conditions. Due to different manufacturers and different types of instruments, the instrument conditions are not the same, so each laboratory should be excellent.
Instrument conditions, 7.1 listed instrument conditions are for reference only.
9.3 The performance of the instrument and graphite tube used and the number of times it is used have an influence on the measurement. The operating conditions of the instrument should be adjusted to the best determination.
status. An atomic absorption spectrometer using a background corrector with a Zeeman or xenon button background. In the measurement process, the selection of the graphite furnace heating program
It is important to choose to prevent splashing of the sample. The resistance value of each graphite tube is different, and the graphite tube has a certain memory effect after use.
The product curve needs to be re-created.
9.4 The injection volume of this method should be determined according to the specific conditions of the instrument, generally choose 10 μL ~ 20 μL.
9.5 Perform interference test of various elements on this method. When the concentration of urinary manganese is 24.5 μg/L to 30.4 μg/L,.2000 μg/L of Pb2,
Cu
2, Co2, Ni2, Cd2, As3, Hg2, Se2, Mg2, Cr6, Na, F-, K, Ca2, Fe2, Cl-, are not measured
Interference.
9.6 Accuracy and precision can be examined when using standard urine samples for quality control samples. Precision can be examined when using contact urine or normal urine.
9.7 Covered wide-mouth polyethylene plastic bottles, volumetric flasks, and colorimetric tubes are required to be soaked overnight in a 1.1 nitric acid solution, followed by water,
Wash with deionized water.
9.8 Laboratory supplies should be tested by adding 1% nitric acid solution as the liquid to be tested. The test result should be less than the detection limit.
9.9 Quality control of the testing process shall be carried out in accordance with the requirements of GBZ /T 295.
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