GBZ/T 307.2-2018Determination of cadmium in urine -- Part 2: Inductively coupled plasma mass spectrometry method (English PDF)

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.

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 (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, rho20=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

8 Calculation

Calculate the concentration of cadmium in the urine sample according to formula (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.