Search result: GBZT307.2-2018
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Determination of cadmium in urine -- Part 2: Inductively coupled plasma mass spectrometry method
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GBZ/T 307.2-2018
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| Standard ID | GBZ/T 307.2-2018 (GBZ/T307.2-2018) | | Description (Translated English) | Determination of cadmium in urine -- Part 2: Inductively coupled plasma mass spectrometry method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | C60 | | Word Count Estimation | 6,633 | | Date of Issue | 2018-08-16 | | Date of Implementation | 2019-01-01 | | Regulation (derived from) | State-Health-Communication (2018) No.14 |
GBZ/T 307.2-2018
Determination of cadmium in urine - Part 2. Inductively coupled plasma mass spectrometry method
ICS 13.100
C 52
Determination of cadmium in urine
Part 2. Inductively coupled plasma mass spectrometry
Determination of cadmium in urine-
Part 2. 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
National Occupational Health Standards
Foreword
This standard is formulated in accordance with the Law of the People's Republic
GBZ /T 307 "Determination of cadmium in urine" is divided into two parts.
-- Part 1. Graphite furnace atomic absorption spectrometry;
-- Part 2. Inductively coupled plasma mass spectrometry.
This part is the second part of GBZ /T 307.
This part is drafted in accordance with the rules given in GB/T 1.1-2009.
This section is mainly drafted by. China Center for Disease Control and Prevention, Occupational Health and Poison Control Institute, Guangdong Provincial Occupational Disease Prevention and Treatment Institute, Jiangsu
Provincial Center for Disease Control and Prevention, Shandong Institute of Occupational Health and Occupational Diseases.
The main drafters of this section. Pan Yajuan, Ding Chunguang, Zhang Aihua, Dong Ming, Zhu Alco, Liu Dezhen, Xu Guang.
Determination of cadmium in urine - Part 2. Inductively coupled plasma mass spectrometry
1 Scope
This part of GBZ /T 307 specifies inductively coupled plasma mass spectrometry for the determination of cadmium in urine.
This section applies to the determination of cadmium in 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 directly diluted with 0.5% nitric acid solution, with 铑 (Rh, 10.0 μg/L) as an internal standard, with inductance
The concentration of cadmium in the diluent was determined by coupled plasma mass spectrometry.
4 instruments
4.1 Covered polyethylene plastic bottle. 100 mL.
4.2 Volumetric flask. 10 mL.
4.3 Polyethylene centrifuge tube. 15 mL.
4.4 Micropipette. The range is from 100 μL to 1000 μL.
4.5 Inductively Coupled Plasma Mass Spectrometer. equipped with an autosampler.
Instrument operation reference conditions.
a) cooling gas flow rate. 12.5 L/min;
b) auxiliary gas flow rate. 0.70 L/min;
c) atomizing gas flow rate. 0.88 L/min;
d) peristaltic pump speed. 30 r/min;
e) Nebulizer temperature. 3 °C.
Note. The above conditions are provided for the convenience of standard users. If the conditions are changed, the same effect should be achieved.
5 reagent
5.1 Deionized water.
5.2 Nitric acid, excellent grade pure, ρ20=1.42 g/mL.
5.3 Nitric acid solution, 0.5% (volume fraction).
5.4 Blank urine sample. Normal human urine that does not touch cadmium, add nitric acid in a ratio of 100 1 and mix.
5.5 Standard solution. Adopt nationally recognized standard solution of cadmium and strontium.
6 Sample collection, transportation and storage
6.1 Collect 100 mL of urine sample in polyethylene plastic bottle, add nitric acid in a ratio of 100.1, mix well, and measure urinary muscle as soon as possible.
anhydride.
6.2 Sample blank. randomly take 2 parts of the urine collection container with the same batch number as the sample collection, and add water equivalent to the sample collection amount as the sample.
Blank, transport and save at the same time as the sample.
6.3 Sample transportation. Store the collected samples and sample blanks in a clean container for refrigerated transport.
6.4 Sample storage. Store at 4 °C for 2 months.
7 Analysis steps
7.1 Preparation of urinary cadmium standard series
The cadmium monolith standard solution was diluted to 1.0 μg/mL cadmium standard application solution with 0.5% nitric acid solution, and then the concentration was 0.0 μg/L.
0.2 μg/L, 1.0 μg/L, 5.0 μg/L, 10.0 μg/L, 20.0 μg/L cadmium standard solution series (medium is 0.5% nitric acid solution).
7.2 Pretreatment of urinary cadmium samples and sample blanks
Remove the urinary cadmium sample or sample blank and return to the laboratory temperature. Shake well and mix well, take 0.50 mL, and place in 15 mL polyethylene
In the centrifuge tube, add 4.50 mL of 0.5% nitric acid solution and shake it to be tested. The rest of the treatment steps are the same as above. At the same time as a reagent blank, the same sample
deal with.
7.3 Determination of urinary cadmium standard series, samples and sample blanks
7.3.1 Determination of urinary cadmium standard series. The instrument was adjusted to the best measurement state, and each standard solution was determined, and each concentration was repeatedly measured twice.
The working curve is plotted against the corresponding cadmium concentration (μg/L) or the regression equation is calculated.
7.3.2 Determination of sample and sample blanks. Determine the sample and sample blanks using the operating conditions of the measurement work series, and subtract the measured count value.
After the reagent blank count value, the cadmium concentration (μg/L) was calculated from the standard curve or the regression equation.
7.4 Quality control of the inspection process
7.4.1 The blank measurement result should be less than the detection limit. When the test result is greater than the detection limit, it indicates that the sample is in the process of collection, transportation and storage.
If contaminated, batch samples should be discarded.
7.4.2 Before the urine sample is tested, two levels of urinary cadmium quality control samples shall be measured simultaneously. The quality control sample is processed and sampled.
Processing should be carried out in the same batch. After measuring the standard series of urinary cadmium and drawing a standard curve, first measure the quality control sample, such as the quality control sample.
The determination results fall within a given range and sample determination can be performed. The quality control sample should be repeatedly determined after every 10 samples were measured. When the measurement result
When the given range is exceeded, the first 10 samples should be re-measured.
8 calculation
Calculate the concentration of cadmium in the urine sample according to formula (1).
Cr
FC
(1)
In the formula.
C - the concentration of cadmium in urine, in micrograms per gram of creatinine (μg/g creatinine);
C0 - the concentration of cadmium in the urine sample obtained from the working curve or the regression equation in micrograms per liter (μg/L);
F - sample dilution factor.
Cr - Urinary creatinine concentration in grams per liter (g/L).
9 Description
9.1 The detection limit of this method is 0.08 μg/L, the lower limit of quantification is 0.30 μg/L; the measurement range is 0.30 μg/L to.200.0 μg/L. relatively
The standard deviation ranges from 1.0% to 1.6% (n=6).
9.2 Volumetric flasks and other supplies need to be soaked overnight in 1..1 nitric acid solution, washed sequentially with tap water, laboratory water, and added
The background test is carried out by using 1% nitric acid solution as the method to be tested, and the test result should be less than the detection limit. Covered polyethylene plastic bottle with stoppered polyethylene
Disposable products such as centrifuge tubes and micro-pump tips should also be used after sampling.
9.3 The quality control of the testing process shall be carried out in accordance with the requirements of GBZ /T 295.
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