HJ 602-2011_English: PDF (HJ602-2011)
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Water quality. Determination of barium. Graphite furnace atomic absorption spectrophotometry
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HJ 602-2011
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Standards related to: HJ 602-2011
| Standard ID | HJ 602-2011 (HJ602-2011) | | Description (Translated English) | Water quality. Determination of barium. Graphite furnace atomic absorption spectrophotometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 12,128 | | Date of Issue | 2011-02-10 | | Date of Implementation | 2011-06-01 | | Quoted Standard | HJ/T 91; HJ/T 164 | | Drafting Organization | Changchun Municipal Environmental Monitoring Center Station | | Administrative Organization | Ministry of Environment Protection | | Regulation (derived from) | Department of Environmental Protection Notice No. 9 of 2011 | | Summary | This standard specifies the determination of barium graphite furnace atomic absorption spectrophotometry. This standard applies to surface water, groundwater, industrial wastewater and domestic sewage and total soluble barium barium determination. | HJ 602-2011
Water quality.Determination of barium.Graphite furnace atomic absorption spectrophotometry
National Environmental Protection Standard of the People's Republic
Determination of water quality
Graphite furnace atomic absorption spectrophotometry
Water quality-Determination of barium
-Graphite furnace atomic absorption spectrophotometry
Published on.2011-02-10
2011-06-01 Implementation
Ministry of Environmental Protection released
Ministry of Environmental Protection
announcement
No. 9 of.2011
In order to implement the "Environmental Protection Law of the People's Republic of China", protect the environment, protect human health, and standardize environmental monitoring, the water is now approved.
The determination of total mercury is determined by the Cold Atomic Absorption Spectrophotometry and other nine standards for national environmental protection standards.
The standard name and number are as follows.
I. Determination of total mercury in water - Cold atomic absorption spectrophotometric method (HJ 597-2011);
2. Determination of water quality ladders by sodium sulfite spectrophotometry (HJ 598-2011);
3. Determination of water quality ladders N-chlorohexadecylpyridine-sodium sulfite spectrophotometry (HJ 599-2011);
4. Gas chromatographic method (HJ 600-2011) for the determination of water quality ladders, black ropes, and dien ladders;
5. Determination of water quality of formaldehyde - Acetylacetone spectrophotometry (HJ 601-2011);
VII. Determination of water quality 火焰 Flame atomic absorption spectrophotometry (HJ 603-2011);
VIII. Determination of total hydrocarbons in ambient air - Gas chromatography (HJ 604-2011);
IX. Determination of Volatile Organic Compounds in Soils and Sediments Purge and Trap/Gas Chromatography-Mass Spectrometry (HJ 605-2011).
The above standards have been implemented since June 1,.2011 and published by the China Environmental Science Press. The standard content can be found on the website of the Ministry of Environmental Protection.
From the date of implementation of the above standards, the following seven national environmental protection standards approved and issued by the former National Environmental Protection Agency shall be abolished.
The name and number are as follows.
1. Determination of total mercury in water quality by cold atomic absorption spectrophotometry (GB 7468-87);
2. Determination of water quality ladders by sodium sulfite spectrophotometry (GB/T 13905-92);
3. Determination of water quality ladders by spectrophotometry (GB/T 13903-92);
4. Determination of water quality TNT, Hessian and Dien, gas chromatography (GB/T 13904-92);
V. Determination of water quality formaldehyde acetylacetone spectrophotometry (GB 13197-91);
6. Determination of water quality 原子 Atomic absorption spectrophotometry (GB/T 15506-1995);
VII. Determination of total hydrocarbons in ambient air Gas chromatography (GB/T 15263-94).
Special announcement.
February 10,.2011
Content
Foreword..iv
1 Scope..1
2 Normative references..1
3 Terms and Definitions.1
4 method principle..1
5 Interference and elimination.1
6 reagents and materials. 2
7 instruments and equipment.2
8 samples. 2
9 Analysis steps..3
10 result calculation and representation 4
11 Precision and Accuracy 4
12 Quality Assurance and Quality Control.5
13 Notes 5
Appendix A (Normative Appendix) Standard Addition Method..6
Appendix B (informative) Applicability judgment of the standard addition method 7
Appendix C (informative) Treatment methods for tungsten and tantalum metal coated graphite tubes..7
Iv
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
This standard is established for the determination of the health and standardization of strontium in water.
This standard specifies the graphite furnace atomic absorption spectrophotometry for the determination of bismuth in water.
This standard is the first release.
Appendix A of this standard is a normative appendix, and Appendix B and Appendix C are informative appendices.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. Changchun Environmental Monitoring Center Station.
This standard is verified by. Shenyang Environmental Monitoring Center Station, Dalian Environmental Monitoring Center, Jilin Province Environmental Monitoring Center Station, Harbin
Municipal Environmental Monitoring Center Station, Technical Center of Jilin Entry-Exit Inspection and Quarantine Bureau and Jilin Province Product Quality Supervision and Inspection Institute.
This standard was approved by the Ministry of Environmental Protection on February 10,.2011.
This standard has been implemented since June 1,.2011.
This standard is explained by the Ministry of Environmental Protection.
Water quality 钡 Determination of graphite furnace atomic absorption spectrophotometry
1 Scope of application
This standard specifies the graphite furnace atomic absorption spectrophotometry for the determination of bismuth in water.
This standard applies to the determination of soluble strontium and total strontium in surface water, groundwater, industrial wastewater and domestic sewage.
When the injection volume is 20.0 μl, the detection limit of this method is 2.5 μg/L, and the lower limit of determination is 10.0 μg/L.
2 Normative references
The contents of this standard refer to the following documents or their terms. For undated references, the valid version applies to this standard.
quasi.
HJ/T 91 Surface Water and Wastewater Monitoring Technical Specifications
HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring
3 Terms and definitions
The following terms and definitions apply to this standard.
3.1
Soluble 钡soluble barium
Refers to the enthalpy determined after filtration of a non-acidified sample through a 0.45 μm filter.
3.2
Total quantity of barium
Refers to the enthalpy determined after digestion of the unfiltered sample.
4 Principle of the method
The sample is filtered or digested and injected into a graphite furnace atomizer. The helium ions are atomized in the graphite tube by high temperature, and the ground state atoms are hollowed out.
The characteristic line emitted by the cathodic lamp emits selective absorption at 553.6 nm, and its absorbance value is proportional to the mass concentration of erbium.
5 interference and elimination
5.1 The concentration of potassium, sodium and magnesium in the sample is 500 mg/L, chromium is 10 mg/L, manganese is 25 mg/L, iron and zinc are 2.5 mg/L, aluminum
When it is 2 mg/L and the nitric acid is 5% (volume fraction) or less, there is no influence on the measurement of hydrazine. When the mass concentration of these substances exceeds the above quality
At the concentration, the standard addition method can be used to eliminate the interference, see Appendix A. The applicability of the standard addition method is judged in Appendix B.
5.2 When the mass concentration of calcium in the sample is greater than 5 mg/L, it will cause positive interference to the determination of strontium. When the mass concentration of calcium in the atomizer is
When 100～300 mg/L, the interference of calcium on strontium does not change with the change of calcium concentration. According to the interference characteristics of calcium, the chemical improver nitric acid is added.
Calcium solution (6.9) can both eliminate the memory effect and increase the sensitivity of the assay. If the mass concentration of calcium in the sample exceeds 300 mg/L, it should be
The sample was appropriately diluted and measured.
6 reagents and materials
Analytically pure reagents in accordance with national standards were used for analysis, unless otherwise stated. The experimental water was deionized water or water of equivalent purity.
6.1 Concentrated nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure.
6.2 Nitric acid solution. 0.5% (volume fraction), prepared with concentrated nitric acid (6.1).
6.3 Concentrated nitric acid. ρ (HNO3) = 1.42 g/ml.
6.4 Nitric acid solution. 19. Prepared with concentrated nitric acid (6.3).
6.5 Barium nitrate [Ba(NO3)2]. Spectral purity.
6.6 钡 standard stock solution. ρ (Ba) = 1 000 mg/L.
Accurately weigh 0.190 3 g lanthanum nitrate (6.5), dissolve it with nitric acid solution (6.2) and dilute to 100 ml, mix. Or buy a city
Standard materials are sold.
6.7 钡 standard intermediate solution. ρ (Ba) = 50.0 mg/L.
Accurately measure 5.00 ml of standard stock solution (6.6) in a 100 ml volumetric flask, dilute to the mark with nitric acid solution (6.2), and mix.
Stored in a polyethylene bottle and stored for 30 days at 4 °C.
6.8 钡 Standard use solution. ρ (Ba) = 1.0 mg/L.
Accurately measure 2.00 ml of 钡 standard intermediate solution (6.7) in a 100 ml volumetric flask and dilute to the mark with nitric acid solution (6.2).
Mix well.
6.9 Calcium nitrate solution. ρ (Ca) = 500 mg/L.
Accurately weigh 2.95 g of calcium nitrate [Ca(NO3)2·4H2O], dissolve it with nitric acid solution (6.2) and dilute to a volume of 1 000 ml, and mix.
6.10 Argon. purity ≥ 99.9%.
7 Instruments and equipment
7.1 Graphite furnace atomic absorption spectrophotometer.
7.2 Electric heating plate.
7.3 Filter unit with a pore size of 0.45 μm acetate or polyethylene filter.
7.4 Vial, 500 ml, made of polyethylene.
7.5 Common instruments and equipment used in general laboratories.
8 samples
8.1 Sample collection
Samples were collected according to the relevant regulations of HJ/T 91 and HJ/T 164, and samples of soluble sputum and total sputum should be collected separately.
8.2 Preservation of samples
8.2.1 Soluble bismuth sample
After the sample is collected, it should be filtered by a suction device as soon as possible, and the initial filtrate is discarded. Collect 100 ml of the filtrate in the vial and add 0.5 ml
Concentrated nitric acid (6.1), stored at 4 ° C in cold storage, measured within 14 days.
8.2.2 Total sample
After sample collection, it should be acidified to pH ≤ 2 by adding concentrated nitric acid (6.1), stored at 4 ° C in cold storage, and measured within 14 days.
8.3 Preparation of samples
8.3.1 Soluble bismuth sample
Accurately measure 40.0 ml of sample (8.2.1) in a 50 ml volumetric flask, dilute to volume with calcium nitrate solution (6.9), shake well.
To be tested.
8.3.2 Total sample
Accurately measure 50.0 ml of the shaken sample (8.2.2) in a Teflon beaker and add 3 to 5 ml of concentrated nitric acid (6.1).
Heat on a hot plate to keep the solution from boiling (about 95 ° C) and steam to about 5 ml. If the solution is turbid, add 2 ml of concentrated nitric acid (6.1).
Continue heating until the solution is clear. The beaker was removed and cooled for 1 min, and 20 ml of nitric acid solution (6.2) was added to the hot plate to continue heating (60~
70 ° C) until the residue is dissolved. After cooling to room temperature, transfer the solution to a 50 ml volumetric flask, rinse the beaker twice with water, and transfer the eluent to the flask.
Add 10 ml of calcium nitrate solution (6.9) to the volumetric flask, dilute to the mark with nitric acid solution (6.2), shake well, and test.
Note 1. The solution must not be evaporated to dryness during the digestion process. If evaporated, it should be resampled for digestion.
Note 2. When the mass concentration of calcium in the sample is 100-300 mg/L, the soluble strontium or total strontium sample does not need to be added with calcium nitrate solution during the preparation of the sample.
(6.9).
Note 3. When the mass concentration of calcium in the sample exceeds 300 mg/L, dilute the sample with a nitric acid solution (6.2) to make the calcium concentration range 100~
300 mg/L. At this time, the soluble strontium or total strontium sample does not need to be added with a calcium nitrate solution (6.9) during the preparation of the sample.
8.4 Preparation of blank samples
To replace the sample with water, prepare a soluble ruthenium blank sample according to the procedure of 8.3.1, and prepare a total ruthenium blank sample according to the procedure of 8.3.2.
9 Analysis steps
9.1 Instrument Commissioning and Calibration
9.1.1 Reference measurement conditions
Adjust the instrument to the best working condition according to the instrument operating instructions. Refer to Table 1 for the measurement conditions.
Table 1 Reference measurement conditions
Determination element Ba
Light source 钡 hollow cathode lamp
Lamp current/mA 25
Wavelength/nm 553.6
Slit width/nm 0.2
Drying temperature/°C 110
Ashing temperature/° C 1 100
Atomization temperature/° C 2 550
Purification temperature/° C 2 600
Argon flow rate/(ml/min) 250
Injection volume/μl 20.0
9.1.2 Drawing of the calibration curve
Measure 0.00, 0.50, 1.00, 1.50, 2.00, 2.50 ml 钡 standard use solution (6.8) in a 50 ml volumetric flask, respectively
Add 10 ml of calcium nitrate solution (6.9), dilute to the mark with nitric acid solution (6.2), shake well, the standard series mass concentration is 0.0,
10.0, 20.0, 30.0, 40.0, 50.0 μg/L. According to the reference measurement conditions (9.1.1), the measurement is performed from low mass concentration to high quality concentration.
The absorbance of the standard series is corrected by measuring the absorbance at zero concentration as the ordinate and the 钡 content (μg/L) as the abscissa.
9.2 Determination
The absorbance of the sample was measured in the same conditions as in the drawing of the calibration curve.
9.3 Blank test
The absorbance of the blank sample was measured in the same manner as in the measurement (9.2).
10 Calculation and representation of results
10.1 Calculation of results
The mass concentration ρ of the ruthenium in the sample is calculated according to the formula (1).
1 0( ) 1f V
ρ ρρ − × ×= (1)
Where. ρ--the mass concentration of soluble hydrazine or total hydrazine in the sample, μg/L;
1ρ - the mass concentration of soluble cesium or total strontium in the sample obtained from the calibration curve, μg/L;
0ρ -- the mass concentration of soluble cesium or total strontium in the blank sample found on the calibration curve, μg/L;
F--sample dilution ratio;
V1--constant volume, ml;
V--sample volume, ml.
10.2 Results are expressed
When the measurement result is less than 100 μg/L, one decimal place is retained; when the measurement result is greater than 100 μg/L, three significant figures are retained.
11 Precision and accuracy
11.1 Precision
Six laboratories tested the uniform standard solutions with soluble sputum concentrations of 10.0, 20.0 and 25.0 μg/L, respectively.
The indoor relative standard deviations were 2.9% to 5.0%, 1.7% to 3.5%, and 2.3% to 6.4%, respectively. The relative standard deviations between laboratories were
3.4%, 1.2%, 1.4%; repeatability limits were 1.0, 2.1, 2.6 μg/L, respectively; reproducibility limits were 1.3, 2.2, and 3.8 μg/L, respectively.
Six laboratories measured the total actual sample concentration of 13.0, 56.0, and 91.4 μg/L, respectively.
The standard deviations were 8.2% to 11.8%, 3.9% to 5.7%, and 2.1% to 4.1%, respectively; the relative standard deviations between laboratories were 7.6% and 6.0%, respectively.
And 5.5%; the repeatability limits were 3.8, 7.6, and 8.1 μg/L, respectively; the reproducibility limits were 4.3, 9.9, and 15.9 μg/L, respectively.
11.2 Accuracy
Six laboratories measured the uniform standard samples with soluble sputum concentrations of 20.0, 33.0, and 38.0 μg/L, respectively.
The difference is 0.2% to 1.0%, 0.7% to 3.1%, and 0.2% to 1.6%, respectively; the relative error final values are 2.2%±1.7% and 1.5%±1.5%, respectively.
0.8% ± 1.0%.
Six laboratories performed spike analysis on the uniform actual samples with soluble sputum concentrations of 10.6, 14.9, and 25.4 μg/L, respectively.
The spiked mass concentrations were 5.0, 10.0, 20.0 μg/L, and the recoveries were 85% to 97%, 93% to 105%, and 88% to 96%, respectively.
The final recoveries of the spiked recoveries were 91% ± 8.1%, 97% ± 9.9%, and 93% ± 5.5%, respectively.
Six laboratories performed standard addition analysis on the unified actual samples with total mass concentrations of 13.0, 56.0 and 91.4 μg/L, respectively.
The spiked mass concentrations were 5.0, 60.0, and 50.0 μg/L, respectively. The recoveries were 82% to 116%, 87% to 109%, and 88% to 114%, respectively.
The final recoveries of the spiked recoveries were 91% ± 15%, 93% ± 8.8%, and 93% ± 9.9%, respectively.
12 Quality Assurance and Quality Control
12.1 Instrument zero calibration should be performed for every 10 samples analyzed.
12.2 A calibration curve shall be drawn for each sample analyzed and the correlation coefficient shall be greater than or equal to 0.995.
12.3 For every 10 samples, a standard solution of the intermediate point concentration of a calibration curve shall be analyzed, and the measured result is compared with the concentration of the calibration curve at that point.
The deviation should be less than or equal to 10%. Otherwise, the calibration curve needs to be redrawn.
12.4 Each batch of samples should be blanked and the results should be below the method detection limit.
12.5 Each batch of samples shall be tested with at least 10% of parallel samples. When the number of samples is less than 10, at least one parallel sample shall be determined.
The relative deviation should be less than 20%.
12.6 At least 10% of the spiked samples shall be determined for each batch of samples. When the number of samples is less than 10, at least one spiked sample shall be determined and marked back.
The yield should be between 80% and 120%.
13 Precautions
13.1 Glassware, polyethylene containers, etc. used in the experiment should be washed with detergent first, and then soaked in nitric acid solution (6.4) for more than 24 hours.
Wash with tap water and experimental water before use.
13.2 Bismuth is a high-temperature element. It is easy to form hard-dissolving tantalum carbide in ordinary graphite tubes, causing memory effect and making the measurement sensitivity low. build
It is recommended to use high-quality pyrolytic coated graphite tubes or metal coated graphite tubes such as tungsten and tantalum, and the graphite tubes should be air-fired after each sample is analyzed. gold
See Appendix C for the treatment of coated graphite tubes.
Appendix A
(normative appendix)
Standard addition method
A.1 Drawing of the calibration curve
Four equal amounts of the sample to be tested were separately weighed to prepare four solutions of the same total volume. The first part does not add standard solution, 2, 3, 4
The standard solutions of different mass concentrations are added in proportion, and the mass concentrations of the four solutions are ρx, ρx ρ0, ρx 2ρ0, ρx 3ρ0;
The mass concentration of the standard solution ρ0 should be approximately equal to 0.5 times the mass concentration of the sample, that is, ρ0 ≈ 0.5 ρ x . Zero with a blank solution, in the same test
The absorbance of the four solutions was determined in sequence under predetermined conditions. Taking the absorbance as the ordinate, adding the mass concentration of the standard solution to the abscissa, drawing the school
The quasi-curve, the intersection of the curve's reverse extension and the mass concentration axis is the mass concentration of the sample to be tested. This method is only suitable for mass concentration and absorption
A region where the degree is linear. The relationship between the mass concentration of the sample to be tested and the corresponding absorbance is shown in Figure A.1.
Mass concentration/(μg/L) 3ρ02ρ0ρ00ρx
Figure A.1 Relationship between the mass concentration of the element to be tested and the corresponding absorbance
A.2 Precautions
A.2.1 The volume error caused by the addition of the standard solution should not exceed 0.5%.
A.2.2 The standard addition method can only eliminate the influence of the matrix effect and cannot eliminate the influence of background absorption.
Appendix B
(informative appendix)
Judging the applicability of the standard addition method
The absorbance of the sample to be tested was determined to be A, and the mass concentration was found to be x from the calibration curve. Add the standard solution to the sample to be tested, plus
The mass concentration is S, the absorbance is measured as B, and the mass concentration is found from the calibration curve as y. Calculate the sample to be tested according to formula (B.1)
Content c.
Sc
Yx
⎛ ⎞ x= ×⎜ ⎟−⎝ ⎠ (B.1)
When there is a matrix effect, S
Yx− is between 0.5 and 1.5, and standard addition method can be used.
Standard addition method when yx− is outside this range
Not applicable.
Appendix C
(informative appendix)
Treatment method of tungsten and bismuth metal coated graphite tube
The ordinary graphite tube was immersed in a 5% potassium tungstate (or cerium nitrate) solution for 24 hours, and then taken out and dried in an oven at 105 ° C for 2 h.
The filter paper wipes off the salt precipitated on both ends of the graphite tube and is placed in the atomizer. According to 110 ° C (15 s) - 1 100 ° C (20 s) - 2 550 ° C (6 s)
The program is processed 2 to 3 times.
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