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HJ 673-2013Water quality. Determination of vanadium by graphite furnace atomic absorption spectrometric method (English PDF)

水质钒的测定石墨炉原子吸收分光光度法

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Issued by

Ministry of Ecology and Environment

Level / Type

National · Mandatory

Issue date

January 1, 1970

Implementation date

January 1, 1970

Scope

HJ 673-2013 is the English-translated version of 水质钒的测定石墨炉原子吸收分光光度法.

HJ 673-2013 — This standard specifies the graphite furnace atomic absorption spectrophotometry for the determination of vanadium in water and wastewater. This standard applies to the determination of vanadium in surface water, groundwater, domestic sewage and industrial wastewater.

The detection limit of this method is 0.003 mg/L, the lower limit of determination is 0.012 mg/L, and the upper limit of determination is 0.200 mg/L.

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Document preview — HJ 673-2013

National Standard of the People's Republic of China

ICS: 13.060
Classification: Z 16
Replacing: GB/T 14673-1993

Issued by: Ministry of Ecology and Environment

Foreword
1 Scope of application
2 Principle of the method
3 Interference and elimination
4 Reagents and materials
5 Instruments and equipment
6 Samples
6.1 Sample collection and preservation
7.1 Commissioning of the instrument
7.2 Calibration
7.3 Sample determination
8 Calculation of results
8.1 Calculation of results
8.2 Results representation
9 Precision and accuracy
9.1 Precision
9.2 Accuracy
10 Quality Assurance and Quality Control
11 Waste disposal

Foreword

To protect the environment and protect the human body in order to implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on Water Pollution Prevention and Control Health, standardization of vanadium monitoring methods in water, revision of this standard.

This standard specifies the graphite furnace atomic absorption spectrophotometry for the determination of vanadium in water and wastewater.

This standard applies to the determination of vanadium in surface water, groundwater, domestic sewage and industrial wastewater.

This standard is a revision of the "Glass furnace atomic absorption spectrophotometry" (GB/T 14673-1993). This standard First published in 1993. The original standard was drafted by. Shanghai Environmental Monitoring Center. This is the first revision.

The main revisions are as follows.

-- Added common elements and concentration-related content of anti-interference in this standard method;

-- Modified the detection limit and lower limit of determination of vanadium;

-- Rewritten the original standard Chinese character expression and standard format.

From the date of implementation of this standard, "Determination of water quality vanadium by graphite furnace atomic absorption spectrophotometry" (GB/T 14673-1993) is abolished.

This standard is revised and revised by the Science and Technology Standards Department of the Ministry of Environmental Protection.

This standard is mainly drafted by. National Environmental Analysis and Testing Center.

The units that participate in the verification of this standard are. National Environmental Analysis and Testing Center, Beijing Physical and Chemical Testing Center, and Heilongjiang Environmental Monitoring Center.

Harbin Environmental Monitoring Center, Guangxi Environmental Monitoring Center, Yinchuan Environmental Monitoring Center.

This standard was approved by the Ministry of Environmental Protection on November 21, 2013.

This standard has been implemented since February 1, 2014.

This standard is explained by the Ministry of Environmental Protection.

Water quality - Determination of vanadium - Graphite furnace atomic absorption spectrophotometric method

1 Scope of application

This standard specifies the graphite furnace atomic absorption spectrophotometry for the determination of vanadium in water and wastewater.

This standard applies to the determination of vanadium in surface water, groundwater, domestic sewage and industrial wastewater.

The detection limit of this method is 0.003 mg/L, the lower limit of determination is 0.012 mg/L, and the upper limit of determination is 0.200 mg/L.

2 Principle of the method

After proper processing, the sample is injected into a graphite furnace atomizer. The vanadium ions contained in the sample are atomized in the graphite tube, which is high.

The temperature is separated into atomic vapor. The ground state atom of the element to be tested absorbs the resonance line energy from the vanadium hollow cathode lamp.

Its absorbance is proportional to its concentration within a certain range.

3 Interference and elimination

The common coexisting components in surface water and groundwater do not interfere with the determination of vanadium.

Coexisting ions and compounds in industrial wastewater do not interfere with the determination at common concentrations. When the wastewater contains 0.040 mg/L Vanadium, 10,000 mg/L Cl, 300 mg/L Fe, 100 mg/L Co, Zn, Mn, K, Na, Ca, Mg, Sb, Bi, Pb, 10.0 mg/L of Ni, Cu, Cr, Cd, As, Ag had no effect on the measurement results.

4 Reagents and materials

The reagents used in this standard are analyzed using analytical reagents in accordance with national standards, unless otherwise stated.

The water is freshly prepared deionized or distilled water.

4.1 Nitric acid (HNO3). rho = 1.42 g/mL, excellent grade pure.

4.2 Ammonium metavanadate (NH4VO3). spectrally pure.

4.3 Nitric acid solution. 1 1. Formulated with nitric acid (4.1).

4.4 Nitric acid solution. 0.2 99.8. Formulated with nitric acid (4.1).

4.5 Standard stock solution of vanadium. rho=1000 mg/L.

Weigh 2.960g (am. accurate to 0.0001g) of ammonium metavanadate (4.2), dissolve with 5mL nitric acid (4.1), and heat if necessary.

Until completely dissolved, dilute to 1000 mL with water. Or purchase certified standard samples.

4.6 Standard use solution of vanadium. rho=0.200 mg/L.

Prepare by diluting the vanadium standard stock solution (4.5) with a nitric acid solution (4.4).

4.7 Argon, purity not less than 99.99%.

5 Instruments and equipment

Unless otherwise stated, the analysis used a Class A glass gauge in accordance with national standards.

5.1 Graphite furnace atomic absorption spectrophotometer with background correction function.

5.2 Pyrolytic coated graphite tube.

5.3 Vanadium hollow cathode lamp.

5.4 Common instruments and common glassware in general laboratories.

6 Samples

6.1 Sample collection and preservation

Samples were taken in polyethylene plastic bottles. Wash the polyethylene plastic bottle 3 times before sampling. Sample collection when determining the total amount of vanadium Immediately after the addition of nitric acid (4.3), the pH was adjusted to 7 Analysis steps

7.1 Commissioning of the instrument

The measurement parameters can be selected according to the instrument's instruction manual. Table 1, Table 2 lists the instrument reference measurement parameters.

Table 1 Instrument reference measurement conditions

Element wavelength (nm) lamp current (mA) slit (nm) V 318.4 12.5 1.3

Table 2 Reference temperature program

Heating stage temperature (°C) time (s) Dry 80~140 20 Ashing 900 20 Atomization 2700 6 Clear 2800 4

7.2 Calibration

Add 0, 2.00, 4.00, 6.00, 8.00, 10.0 mL vanadium standard solution (4.6.3) to a 10 mL volumetric flask.

Make up the nitric acid solution (4.4) to the mark. The concentrations are 0, 40.0, 80.0, 120, 160,.200 µg/L, respectively. Take 20µL mark for the quasi-series solution samples, the absorbance is measured in order from the low to the high concentration according to the instrument parameters set in (7.1).

The calibration curve was established by taking the vanadium standard solution concentration (µg/L) as the abscissa and the absorbance measurement value as the ordinate. Linear back the analysis method determines the slope for the sample content calculation.

7.3 Sample determination

A 20 µL sample was taken and the absorbance was measured under the same conditions as in (7.2). Vanadium was obtained from the absorbance value from the calibration curve regression equation content. When the vanadium content exceeds the measurement range of the calibration curve, the water sample can be diluted and measured.

8 Calculation of results

8.1 Calculation of results

The concentration of vanadium in the water sample is calculated as follows.

Vk )( rhorhorho

Where rho - the concentration of vanadium in the water sample, mg/L;

k -- dilution ratio of water sample;

rho1 - the vanadium concentration in the test solution obtained from the calibration curve regression equation, µg/L;

rho0 -- the vanadium concentration in the sample blank obtained from the calibration curve regression equation, µg/L;

V1 - volume of volume before water sample measurement, mL;

V - water sample volume, mL.

8.2 Results representation

The result indicates whether the sample test item is dissolved vanadium or vanadium. When the result is greater than 1 mg/L, the calculation result is 3 the effect number, when the result is less than 1 mg/L, the number after the decimal point is retained to the third place.

9 Precision and accuracy

9.1 Precision

Six laboratories sampled uniform vanadium-containing industrial wastewater with mass concentrations of 18.5µg/L, 58.0µg/L, and 143 µg/L.

The measurement was taken. The relative standard deviations in the experimental room were 1.30~4.11 (%), 0.59~2.42 (%), 0.40~2.06 (%), respectively.

The relative standard deviations between the laboratories were 7.03%, 4.02%, and 7.69%, respectively. Reproducibility limits are 1.4µg/L, 2.3 µg/L and 4.9 Gg/L. The reproducibility limits were 3.6 µg/L, 6.5 µg/L, and 31 µg/L, respectively.

9.2 Accuracy

Six laboratories tested the certified vanadium standard samples with a mass concentration of 233±11 (µg/L). The relative error results ranged from-0.07~2.65 (%).

Six laboratories carried out spiked recovery experiments on surface water samples. When the spiked concentration was 10.0 µg/L, the spiked recovery rate was the circumference is 94.1%~102 (%); the final recovery of the spiked standard is 98.1±4.6 (%). The total vanadium concentration is 18.5 µg/L, 58.0 µg/L industrial wastewater samples were spiked and analyzed, and the spiked concentrations were 20.0 µg/L and 80.0 µg/L, respectively.

The yield results ranged from 94.6 to 103 (%); 93.6 to 104.0 (%); the final recoveries were 98.7 ± 5.6 (%), respectively.

99.5 ± 5.6 (%).

10 Quality Assurance and Quality Control

10.1 Glassware commonly used in laboratories should be soaked in nitric acid (4.3) for 24 hours, washed with water and set aside.

10.1 For each batch of water sample (<=10), two laboratory reagent blanks should be made. If the blank sample response is high, you should be careful Find the reason and eliminate the factor of high blank value.

10.2 There should be a sample spike test for each sample of the same type to determine if matrix interference is present. Recovery rate quality control index Between 90 and 110 (%). Samples from different sources should be considered for addition to the sample spike test.

10.3 There should be one parallel sample for each batch (<=10) of samples analyzed. When the quantity is large, the number of parallel samples should be selected in proportion to 10%.

The deviation of the parallel sample results should be less than the repeatability limit.

10.4 For each 10 samples measured, one calibration curve check point should be measured (take the middle concentration of the calibration curve), and its concentration value for comparison, the relative deviation should be within 10%. If the measurement result of the calibration sample exceeds this range, it should be re-measured and produced.

Calibrate the curve and review the measured samples.

10.5 The correlation coefficient of the calibration curve regression equation for each production should be greater than 0.999.

11 Waste disposal

The waste liquid produced in the experiment should be adjusted to alkaline, and then stored with sodium sulfide and stored, and then sent to qualified units.

deal with.

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 7 pages — is available in the English PDF.

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