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GBZT303-2018: Determination of lead in urine -- Graphite furnace atomic absorption spectrometry method
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Determination of lead in urine -- Graphite furnace atomic absorption spectrometry method
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GBZ/T 303-2018
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Basic data | Standard ID | GBZ/T 303-2018 (GBZ/T303-2018) | | Description (Translated English) | Determination of lead in urine -- Graphite furnace atomic absorption spectrometry method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | C60 | | Word Count Estimation | 7,730 | | Date of Issue | 2018-08-16 | | Date of Implementation | 2019-01-01 | | Older Standard (superseded by this standard) | WS/T 18-1996 | | Regulation (derived from) | State-Health-Communication (2018) No.14 | | Issuing agency(ies) | National Health and Family Planning Commission | GBZ/T 303-2018: Determination of lead in urine -- Graphite furnace atomic absorption spectrometry method
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Determination of lead in urine - Graphite furnace atomic absorption spectrometry method
ICS 13.100
C 52
National Occupational Health Standards
Replace WS/T 18-1996
Determination of lead in urine - Graphite furnace atomic absorption spectrometry
Determination of lead 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
Foreword
This standard is formulated in accordance with the Law of the People's Republic
This standard replaces WS/T 18-1996 "Method for the determination of lead in urine by graphite furnace atomic absorption spectrometry".
Compared with WS/T 18-1996, the main changes are as follows.
----The operating conditions of the instrument are changed to the reference conditions for instrument operation;
---- Improved matrix modifier, standard preparation, and measurement range;
---- Added the requirement for sample dilution.
This standard 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, Shandong
Provincial Institute of Labor Health and Occupational Diseases, Jiangsu Provincial Center for Disease Control and Prevention.
The main drafters of this standard. Zhang Jing, Zhang Aihua, Xu Guang, Zhu Alcohol, Zhang Zhihu.
The previous versions of the standards replaced by this standard.
--WS/T 18-1996.
Determination of lead in urine - Graphite furnace atomic absorption method
1 Scope
This standard specifies the graphite furnace atomic absorption method for the determination of lead in urine.
This standard applies to the determination of lead in urine in occupational exposure personnel.
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
GB/T 6682 Analytical laboratory water specifications and experimental methods
3 Principle
Urine sample (hereinafter referred to as urine sample) with palladium chloride matrix modifier, measured by graphite furnace atomic absorption spectrometry at 283.3 nm
Determine the concentration of lead.
4 instruments
4.1 Covered polyethylene plastic bottle, 100 mL.
4.2 stoppered polyethylene centrifuge tube, 1.5 mL.
4.3 Volumetric flask, 10 mL.
4.4 Microsampler,.200 μL, 1000 μL.
4.5 Atomic absorption spectrophotometer with graphite furnace, background correction and lead hollow cathode lamp. 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
Dry 90 1 30 250
Dry 120 15 30 250
Ashing 800 10 20 250
Atomic 1900 0 5 0
Clear 2100 1 3 250
5 reagent
5.1 Experimental water. According to GB/T 6682.
5.2 Nitric acid, ρ20=1.42 g/mL, excellent grade pure.
5.3 Nitric acid solution, 1% (volume fraction).
5.4 Matrix modifier. 0.33 g of palladium chloride (excellent grade) is slightly soluble in 10 mL of nitric acid, shake well, and diluted to 500.0 mL with water. Storage
Stored in a brown reagent bottle and stored in the refrigerator for one year.
5.5 Normal human urine. normal human urine that does not touch lead.
5.6 Lead standard solution. The lead standard solution standard substance with the national standard substance certificate number is used.
5.7 Lead Standard Application Solution. Dilute the lead standard solution to 1.0 μg/mL lead standard application solution with 1% nitric acid.
6 Sample collection, transportation and storage
6.1 Sample collection. Collect about 50 mL of urine sample once in a polyethylene plastic bottle. After measuring the specific gravity as soon as possible, add in proportion to 1%
Nitric acid, mix well.
6.2 Sample blank. Take 5 mL of 1% nitric acid in a plastic tube with a blank.
6.3 Samples and sample blanks should be placed in a clean container and shipped under refrigerated conditions. It can be stored in the refrigerator at -18 ° C for 1 month.
7 Analysis steps
7.1 Preparation of the standard series of lead working curves
Take 7 10 mL volumetric flasks and add 0.00 mL, 0.20 mL, 0.40 mL, 0.80 mL, 1.20 mL, 1.60 mL, 2.00 mL, respectively.
Lead standard application solution, each with palladium chloride matrix modifier to 10 mL, configured to be 0.0 μg/L, 20.0 μg/L, 40.0 μg/L, 80.0 μg/L,
120.0 μg/L, 160.0 μg/L,.200.0 μg/L lead standard series, see Table 2.
Table 2 Preparation of the standard series of lead working curves
Pipe number 0 1 2 3 4 5 6
Lead standard application solution /mL 0.00 0.20 0.40 0.80 1.20 1.60 2.00
Matrix improver /mL 10.0 9.80 9.60 9.20 8.80 8.40 8.00
Lead concentration/(μg/L) 0.0 20.0 40.0 80.0 120.0 160.0.200.0
Before the injection, the lead standard series and the normal human urine sample were processed in the same ratio to prepare a standard series of lead working curves.
7.2 Lead working curve standard series, sample and blank processing method
7.2.1 Lead working curve standard series pretreatment method
0.2 mL of each standard solution was added to a stoppered polyethylene centrifuge tube to add 0.2 mL of normal human urine, and the mixture was mixed for measurement.
7.2.2 Sample pretreatment method
The acidified urine sample was taken out of the refrigerator, and after returning to room temperature, shake well. Pipette 0.2 mL into a stoppered polyethylene centrifuge tube
0.2 mL palladium chloride matrix modifier, mixed for measurement. When the sample concentration exceeds the linear range, the sample should be appropriately diluted and injected.
When diluting the sample, be aware that the sample, blank, and standard series of treatment methods should be consistent. The measurement results do not need to calculate the dilution factor.
7.2.3 Blank Preprocessing Method
0.2 mL of 1% nitric acid was added to a stoppered polyethylene centrifuge tube to add 0.2 mL of palladium chloride matrix modifier, and the mixture was mixed for measurement.
7.3 Determination of lead work curve standard series, samples and blanks
7.3.1 Lead working curve standard series determination
The atomic absorption spectrophotometer is adjusted to the optimum measurement state with reference to the operating conditions of the instrument. Inject 10 μL and measure the suction of each standard tube
Luminosity; after subtracting the absorbance value of tube 0 from the absorbance values of tubes 1 to 6. Drawing a working curve on the lead concentration (μg/L) by absorbance
Calculate the regression equation.
7.3.2 Determination of samples and blanks
The sample solution and the blank solution are determined by the operating conditions of the measurement standard series, and the absorbance value of the sample is subtracted from the absorbance value of the blank,
The working curve or regression equation gives the lead concentration (μg/L) in the urine sample.
7.3.3 Quality Control
According to GBZ /T 173, the freeze-dried human urine lead national standard substance was used as the quality control sample. Quality Control Sample Processing, Determination and Standards
The treatment and measurement of the column and the sample are consistent. A quality control sample is measured before and after the measurement of the sample and between each of the 10 samples to control the sample.
The accuracy of the product inspection.
8 calculation
Calculate the lead concentration of the urine sample according to formula (1).
C = C0 × k (1)
In the formula.
C -- the concentration of lead in urine in micrograms per liter (μg/L);
C0 - the concentration of lead after subtracting the blank from the urine curve obtained by the working curve or the regression equation, in micrograms per liter (μg/L);
k -- The urine sample is converted to the concentration correction factor at the standard specific gravity (1.020).
9 Description
9.1 The minimum detectable concentration of this method is 1.0 μg/L; the lower limit of quantitation is 3.0 μg/L. The measurement range is from 3.0 μg/L to.200 μg/L; batch
The relative standard deviation within the range is 1.0% to 2.6% (n=6), and the relative standard deviation between batches is 1.6% to 3.9% (n=6);
97% to 104.1%.
9.2 Palladium chloride in the matrix modifier used in this method forms a stable complex with lead, and lead is not easily lost during ashing, so ashing
The temperature can be increased to 700 ° C ~ 900 ° C, at which temperature most of the interference components in the urine sample are removed.
9.3 All containers and laboratory supplies should be soaked in a 1.1 nitric acid solution overnight, rinsed with water and distilled water for later use.
9.4 The urine sample collection time is not limited. When the urine sample is taken, it is necessary to leave the site environment, replace the overalls, and do a good job of personal hygiene in a clean room.
Leave urine to prevent lead contamination in the environment.
9.5 When the lead concentration in the urine sample exceeds the measurement range, the working curve range can be increased to 400.0 μg/L, and diluted by 3 times (0.2 mL).
Urine sample, add 0.2 mL matrix modifier plus 0.2 mL 1% nitric acid to mix), 4 fold dilution (0.2 mL urine sample, add 0.2 mL matrix to improve)
Add 0.4 mL of 1% nitric acid to mix) or 5 times to dilute (0.2 mL of urine sample, add 0.2 mL of matrix modifier plus 0.6 mL of 1% nitric acid to mix)
The measurement was carried out. At the same time, the sample, blank and standard series of treatment methods should be consistent. The measurement results do not need to calculate the dilution factor.
9.6 The quality assurance of the entire inspection process shall be carried out in accordance with the requirements of GBZ /T 295.
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