GBZ/T 316.3-2018Determination of lead in blood -- Part 3: Atomic fluorescence spectrometry method (English PDF)

Foreword

This standard is formulated in accordance with the Law of the People's Republic GBZ/T 316-2018 "Determination of lead in blood" is divided into three parts.

-- Part 1. Graphite furnace atomic absorption spectrometry;

-- Part 2. Inductively coupled plasma mass spectrometry;

-- Part 3. Atomic Fluorescence Spectrometry.

This part is the third part of GBZ/T 316.

This part is drafted in accordance with the rules given in GB/T 1.1-2009.

This section drafted by. Beijing Municipal Center for Disease Control and Prevention, China Center for Disease Control and Prevention, Occupational Health and Poison Control Institute, Zhejiang Provincial Academy of Medical Sciences, Kaifeng City Center for Disease Control and Prevention, Henan Province.

1 Scope

This part of GBZ/T 316 specifies atomic fluorescence spectrometry for the determination of lead in blood.

This section applies to the determination of lead in the blood 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

The blood sample (hereinafter referred to as the blood sample) is deproteinized with nitric acid, and the supernatant is taken after centrifugation, and the hydride is reduced to a wavelength of 283.3 nm.

Next, the lead content was measured by an atomic fluorescence spectrometer.

4 Instruments

4.1 Volumetric flask, 10mL.

4.2 stoppered polyethylene centrifuge tube, 5mL.

4.3 High-speed centrifuge, the speed is greater than 10000r/min.

4.4 Vortex mixer.

4.5 Micropipettes, the range is 20µL ~.200µL, 0.5mL ~ 5.0 mL.

4.6 Atomic Fluorescence Spectrometer with high performance lead hollow cathode lamp and hydride generation device.

5 Reagent

5.1 Deionized water.

5.2 Nitric acid, rho20=1.42g/mL, excellent grade pure.

5.3 Nitric acid solution (for sample processing and current carrying), 3.5% (V/V). Dilute 3.5 mL of nitric acid to 100 mL with water.

5.4 sodium hydroxide solution, 30g/L.

5.5 Reducing agent solution. Weigh 10g potassium borohydride (excellent grade pure), dissolve in sodium hydroxide solution, add 20g potassium ferricyanide (analytical grade) and 10 g of boric acid (premium pure), then dissolved in sodium hydroxide solution and diluted to 1000 mL.

5.6 Lead single element standard solution.

6 Sample collection, transportation and storage

According to GBZ/T 295.

The collected samples and sample blanks are placed in a clean container for refrigerated transport.

The sample can be stored for half a year at -20 °C.

7 Analysis steps

8 Calculation

Calculate the concentration of lead in blood according to formula (1).

C = C0×F (1)

In the middle

C - the concentration of lead in the blood, µg/L;

C0--lead concentration from standard curve or regression equation (minus sample blank), µg/L;

F -- sample dilution factor.

9 Description

9.1 The detection limit of this method is 6.7µg/L, and the lower limit of quantification is 20µg/L (according to 0.1mL blood sample, 30 times dilution); the measurement range is 20µg/L ~ 900µg/L; relative standard deviation range of 2.72% ~ 7.01% (n = 6); blood sample spike recovery range of 95.3% ~ 106.0%.

9.2 Adding potassium ferricyanide to the reducing agent can promote the formation of lead hydride; the prepared reducing agent can be stably stored at 4 ° C for 1 week.

9.3 The concentration of nitric acid solution and reducing agent has a great influence on the hydrogenation reaction, and the same batch of samples should be strictly consistent.

9.4 If the lead concentration in the sample exceeds the measurement range, it can be determined by diluting with a nitric acid solution, and multiplying by the corresponding dilution factor.

9.5 This method should strictly control the injection volume, and the injection volume will generate a large number of bubbles during the hydride reaction, which will affect the normal measurement.

9.6 EDTA anticoagulant should not be used for blood collection.

9.7 Quality control of the testing process shall be carried out in accordance with the requirements of GBZ/T 295.