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GBZT307.1-2018 English PDF

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GBZT307.1-2018: Determination of cadmium in urine -- Part 1: Graphite furnace atomic absorption spectrometric method
Status: Valid
Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
GBZ/T 307.1-2018139 Add to Cart 3 days Determination of cadmium in urine -- Part 1: Graphite furnace atomic absorption spectrometric method Valid

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Basic data

Standard ID: GBZ/T 307.1-2018 (GBZ/T307.1-2018)
Description (Translated English): Determination of cadmium in urine -- Part 1: Graphite furnace atomic absorption spectrometric method
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: C60
Word Count Estimation: 7,772
Date of Issue: 2018-08-16
Date of Implementation: 2019-01-01
Older Standard (superseded by this standard): WS/T 32-1996
Regulation (derived from): State-Health-Communication (2018) No.14
Issuing agency(ies): National Health and Family Planning Commission

GBZ/T 307.1-2018: Determination of cadmium in urine -- Part 1: Graphite furnace atomic absorption spectrometric method


---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Determination of cadmium in urine - Part 1. Graphite furnace atomic absorption spectrometric method ICS 13.100 C 52 Replace WS/T 32-1996 Determination of cadmium in urine Part 1. Graphite furnace atomic absorption spectrometry Determination of cadmium in urine- Part 1. 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 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 first part of GBZ /T 307. This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This section replaces WS/T 32-1996 "Method for the determination of cadmium in urine by graphite furnace atomic absorption spectrometry". Compared with WS/T 32-1996, the main changes are as follows. -- The use of new matrix modifiers; -- Improved standard formulation and sample handling methods. 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. The previous versions of the standards replaced by this section. --WS/T 32-1996. Determination of cadmium in urine - Part 1. Graphite furnace atomic absorption spectrometry

1 Scope

This part of GBZ /T 307 specifies a graphite furnace atomic absorption method 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

A urine sample (hereinafter referred to as a urine sample) is diluted with a mixed solution of palladium chloride and nitric acid (ie, a matrix modifier) at a wavelength of 228.8 nm. Next, the concentration of cadmium was determined by graphite furnace atomic absorption spectrometry.

4 instruments

4.1 Covered polyethylene plastic bottle. 100 mL. 4.2 Volumetric flask. 10 mL. 4.3 stoppered polyethylene centrifuge tube. 1.5 mL. 4.4 Micropipette. The range is 20 μL ~.200 μL, 100 μL ~ 1000 μL. 4.5 Atomic Absorption Spectrometer. with graphite furnace, cadmium hollow cathode lamp and background correction device. Refer to Table 1 for instrument operation reference conditions. Table 1 Instrument operation reference conditions step temperature Heating time Residence time Carrier gas flow mL/min Drying 110 5 10 250 Drying 130 10 20 250 Ashing 500 20 30 250 Atomization 1600 0 3 0 Clear 2300 1 5 250 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 Matrix modifier. Weigh 0.20 g of palladium chloride, add slightly heat to 10.0 mL of nitric acid, shake well, and dilute to 500 mL with water. Storage Store in a brown reagent bottle and store it for 1 year in cold storage and protected from light. 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. Use a nationally recognized standard solution. 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. The product is blank and transported and stored 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 working curve solution series Dilute the cadmium monolith standard solution to 100 μg/L urethane cadmium standard application solution with a blank urine sample, and then take 6 10 mL volumetric flasks. No. 1 to 6. Add urinary cadmium standard application solution 0.0 mL, 0.2 mL, 0.5 mL, 0.8 mL, 1.0 mL, 1.5 mL, respectively. The urine sample is fixed to the mark, which is formulated to a concentration of 0.0 μg/L, 2.0 μg/L, 5.0 μg/L, 8.0 μg/L, 10.0 μg/L, and 15.0 μg/L. The urinary cadmium working curve solution series. 7.2 Treatment of urinary cadmium working curve solution series, sample and sample blank 7.2.1 Urinary cadmium working curve solution series treatment. Take 0.20 mL of each concentration of urinary cadmium standard solution in a stoppered polyethylene centrifuge tube, each Add 0.80 mL of matrix modifier to the tube, cover the lid, and mix for measurement. 7.2.2 Sample and sample blank pretreatment. The sample dilution factor is consistent with the dilution factor of the working curve. Refrigerated urine samples and sample blanks Remove and return to laboratory temperature. Shake well and mix well. Take 0.20 mL and place in a 1.5 mL stoppered polyethylene centrifuge tube. The procedure is the same as the standard curve solution. At the same time, the reagent is blank. 7.3 Determination of urinary cadmium working curve solution series, sample and sample blank 7.3.1 Determination of urinary cadmium working curve solution series. Adjust the atomic absorption spectrometer to the best measurement state, and take 15 μL of supernatant to inject. Each standard series was measured, and each concentration was measured three times. After subtracting the absorbance value of No. 1 from the absorbance values of No. 2 to No. 6, the corresponding cadmium is concentrated. Degree (μg/L) plots the working curve or calculates the regression equation. 7.3.2 Determination of sample and sample blanks. Determine the sample and sample blanks by measuring the operating conditions of the standard curve solution series. After subtracting the reagent blank absorbance value from the luminosity value, the concentration of cadmium (μg/L) was calculated from the working curve or the regression equation. 7.4 Quality control of the inspection process 7.4.1 Quality control of the inspection process in accordance with GBZ /T 295. The blank measurement result should be less than the detection limit. When the test result is greater than the checkout The time limit indicates that the sample is contaminated during collection, transportation and storage, and the batch sample 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 urinary cadmium working curve solution series and drawing the working curve, first determine the quality control sample, such as quality control The measurement result of the sample falls within a given range, and the sample can be measured. The quality control sample should be repeatedly determined after every 10 samples were measured. when When the measurement result exceeds the given range, the first 10 samples should be re-measured.

8 calculation

Calculate the concentration of cadmium in the urine sample according to formula (1). Cr  (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); Cr - Urinary creatinine concentration in grams per liter (g/L).

9 Description

9.1 The detection limit of this method is 0.17 μg/L, the lower limit of quantification is 0.50 μg/L; the measurement range is 0.50 μg/L to 15.0 μg/L. relatively The standard deviation ranges from 1.4% to 7.5% (n=6). 9.2 The injection volume of this method can be determined according to the specific conditions of the instrument, generally choose 10 μL ~ 20 μL. 9.3 In this method, the matrix has an influence on the measurement. The sample should be treated in the same way as the working curve series solution. If the cadmium concentration in the sample is super Over the measurement range, the urinary cadmium working curve range can be increased to 30.0 μg/L, urine 0.10 mL, respectively, added 0.90 mL matrix improvement The agent was diluted and measured. When measuring cadmium in normal urine, 0.30 mL of urine can be taken and diluted with 0.60 mL of matrix modifier to determine. 9.4 Volumetric flasks and other supplies should be soaked in a 1.1 nitric acid solution overnight, washed sequentially with tap water, laboratory water, and added with 1% The background test is carried out by using a nitric acid solution as a method to be tested, and the test result should be less than the detection limit. Covered with polyethylene plastic bottle, with polyethylene Disposable items such as heart tube and micropipette tips should also be used after sampling. 9.5 Quality control of the testing process shall be carried out in accordance with the requirements of GBZ /T 295.
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