HJ 1046-2019 English PDF

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HJ 1046-2019: Water quality - Determination of antimony - Flame atomic absorption spectrometry
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Basic data

Standard ID: HJ 1046-2019 (HJ1046-2019)
Description (Translated English): Water quality - Determination of antimony - Flame atomic absorption spectrometry
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z16
Classification of International Standard: 13.060
Word Count Estimation: 13,115
Date of Issue: 2019
Date of Implementation: 2020-04-24
Issuing agency(ies): Ministry of Ecology and Environment

HJ 1046-2019: Water quality - Determination of antimony - Flame atomic absorption spectrometry

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(Water quality-determination of antimony-flame atomic absorption spectrophotometry) National Environmental Protection Standard of the People's Republic of China Determination of water quality antimony Flame atomic absorption spectrophotometry Water quality-Determination of antimony -Flame atomic absorption spectrometry 2019-10-24 released 2020-04-24 Implementation Released by the Ministry of Ecology and Environment

Contents

Foreword ... ii 1 Scope ... 1 2 Normative references ... 1 3 Terms and definitions ... 1 4 Methodology ... 1 5 Interference and cancellation ... 1 6 Reagents and materials ... 2 7 Instruments and equipment ... 2 8 Sample ... 2 9 Analysis steps ... 3 10 Calculation and Representation of Results ... 4 11 Precision and accuracy ... 5 12 Quality Assurance and Quality Control ... 5 13 Waste disposal ... 6 Appendix A (Normative Appendix) Matrix interference inspection methods ... 7 Appendix B (Normative) Standard Addition Method ... 8 Appendix C (Informative) Judgment on the Applicability of Standard Additions ... 9

Foreword

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 Control", protect the ecology Environment, protect human health, standardize the determination method of antimony in water, and formulate this standard. This standard specifies the determination of flame atoms of antimony in high-concentration domestic sewage, industrial wastewater, and relatively polluted surface water. Absorption spectrophotometry. Appendix A and Appendix B of this standard are normative appendixes, and Appendix C is an informative appendix. This standard is issued for the first time. This standard is formulated by the Department of Eco-Environmental Monitoring, Laws and Standards Department of the Ministry of Ecology and Environment. This standard was drafted. Shanghai Pudong New Area Environmental Monitoring Station. Verification units of this standard. Shanghai Environmental Monitoring Center, Shanghai Minhang District Environmental Monitoring Station, Baoshan District, Shanghai Monitoring Station, Shanghai Jiading District Environmental Monitoring Station, Shanghai Qingpu District Environmental Monitoring Station, and Shanghai Huatest Label Testing Technology Limited the company. This standard was approved by the Ministry of Ecology and Environment on October 24,.2019. This standard will be implemented from April 24, 2020. This standard is explained by the Ministry of Ecology and Environment. Water quality--Determination of antimony by flame atomic absorption spectrophotometry Warning. The antimony and its compounds used in the experiment are more toxic, hydrochloric acid is highly corrosive and volatile, and nitric acid is Strongly corrosive and oxidizing, reagent preparation and sample preparation should be carried out in a fume hood, and should be worn as required during operation Protective equipment to avoid contact with skin and clothing.

1 Scope

This standard specifies the flame atomic absorption spectrophotometry for the determination of antimony in water. This standard is applicable to the determination of antimony in high-concentration domestic sewage, industrial wastewater, and surface water that is seriously polluted. The detection limit of the method for the determination of soluble antimony in this standard is 0.2 mg/L, and the lower limit of detection is 0.8 mg/L; the method for the detection of total antimony is The limit is 0.3 mg/L, and the lower limit of determination is 1.2 mg/L.

2 Normative references

This standard refers to the following documents or clauses therein. For undated references, the valid version applies to this standard. HJ/T 91 Technical specifications for surface water and sewage monitoring

3 terms and definitions

The following terms and definitions apply to this standard. 3.1 Soluble antimony Refers to antimony measured after a non-acidified sample is filtered through a 0.45 μm filter. 3.2 Total quantity of antimony Refers to antimony measured after acid filtration of an unfiltered sample.

4 Method principle

After the sample is filtered or digested, it is sprayed into a lean air-acetylene flame. The antimony ground state atom formed in the high-temperature flame is opposite to the light. The characteristic 217.6 nm spectral line emitted from a source (hollow cathode lamp or other light source) produces selective absorption. The absorbance value is directly proportional to the mass concentration of antimony.

5 Interference and cancellation

5.1 The concentration of hydrochloric acid, nitric acid and 2% sulfuric acid below 20% will not interfere with the determination of antimony. 5.2 When the mass concentrations of copper, iron, cadmium, nickel and lead are lower than 3500 mg/L, 4000 mg/L, 1000 mg/L, At 4000 mg/L and 6000 mg/L, it does not interfere with the determination of antimony. For matrix interference inspection, see Appendix A; The entry method can offset the interference, see Appendix B; the applicability judgment of the standard addition method can be found in Appendix C.

6 Reagents and materials

Unless otherwise specified, analytical reagents that meet national standards are used in the analysis, and the experimental water is newly prepared deionized water. Water or water of equivalent purity. 6.1 Hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure. 6.2 Nitric acid. ρ (HNO3) = 1.42 g/ml, excellent purity. 6.3 Nitric acid solution. 1 + 1. 6.4 Nitric acid solution. 1 + 99. 6.5 Tartaric acid. w≥99.5%. 6.6 Metal antimony. w≥99.99%, pure spectrum. 6.7 Antimony standard stock solution. ρ (Sb) = 1000 mg/L. Weigh accurately 1.0 g (accurate to 0.0001 g) metal antimony (6.6), put it in a beaker, add 10 ml hydrochloric acid (6.1) And 20 ml of nitric acid solution (6.3); add 100 ml of water and 1.5 g of tartaric acid (6.5) and warm to completely dissolve. cool down Then transfer it to a 1000 ml volumetric flask, dilute with water to the mark, shake well, transfer to a polyethylene bottle, and seal it. Months. Or use a commercially available certified antimony standard solution. 6.8 Standard solution of antimony. ρ (Sb) = 100.0 mg/L. Accurately transfer 10.00 ml antimony standard stock solution (6.7) into a 100 ml volumetric flask, and dilute with nitric acid solution (6.4). Fill to the mark, shake well, transfer to a polyethylene bottle and seal, and it can be stored for 6 months. 6.9 Gas. acetylene, purity ≥99.6%. 6.10 Assisting gas. air, water, oil and other impurities should be removed before entering the burner. 6.11 Filter. Acetate or PVC filter with a pore size of 0.45 µm.

7 instruments and equipment

7.1 Flame atomic absorption spectrophotometer. 7.2 Light source. Antimony hollow cathode lamp or other light source with 217.6 nm. 7.3 Microwave Digestion Apparatus. 7.4 Electric heating plate. The temperature control range is from room temperature to 300 ° C, and the temperature control accuracy is ± 5 ° C. 7.5 Vial. 500 ml, polyethylene or equivalent. 7.6 Instruments and equipment commonly used in general laboratories.

8 samples

8.1 Sample collection Collect the samples according to the relevant regulations of HJ/T 91. Samples for soluble antimony and total antimony should be collected separately. 8.2 Sample storage 8.2.1 Soluble antimony samples After the sample is collected, it should be filtered with a filter membrane (6.11) as soon as possible. The initial filtrate is discarded, and the required volume of filtrate is collected in a sample bottle. (7.5); add 1 ml of nitric acid (6.2) per 100 ml of filtrate to acidify, and measure within 14 days. 8.2.2 Total antimony samples After sample collection, 1 ml of nitric acid (6.2) was added to every 100 ml sample to acidify it, and it was measured within 14 days. 8.3 Preparation of test specimens 8.3.1 Preparation of soluble antimony samples See 8.2.1. 8.3.2 Preparation of total antimony sample 8.3.2.1 Microwave Digestion Accurately measure 25.0 ml of the total antimony sample (8.2.2) in the digestion tank of the microwave digestion instrument (7.3), add 2.0 ml Nitric acid (6.2) and 6.0 ml hydrochloric acid (6.1) (can reduce or increase the sampling volume and the amount of acid Product), microwave digestion at 170 ° C ± 5 ° C for 10 min. Digestion is complete, after cooling to room temperature, transfer to a 50 ml volumetric flask In water, dilute with water to the mark, shake well, and test. 8.3.2.2 Hot plate digestion method Accurately measure 25.0 ml of the total antimony sample (8.2.2) in a 250 ml Erlenmeyer flask and add 2.0 ml of nitric acid (6.2) And 6.0 ml hydrochloric acid (6.1) (can reduce or increase the sampling volume and the volume of the acid added in proportion to the actual needs), place Cover the watch glass or small funnel on the hot plate (7.4), keep slightly boiling, and stop heating when the sample is uniform and clear, and wait for cooling After reaching room temperature, rinse the inner wall at least 3 times with appropriate amount of water, transfer to a 50 ml volumetric flask, dilute with water to the mark, and shake Uniform, to be tested. 8.4 Preparation of blank samples Use experimental water instead of the sample, and follow the same steps as the sample preparation (8.3) to prepare a laboratory blank sample Equipment.

9 Analysis steps

9.1 Reference measurement conditions The optimal working conditions of different models of instruments are different. You need to adjust the instrument to the best working condition according to the instrument operating instructions. See Table 1 for reference measurement conditions. Table 1 Reference measurement conditions Wavelength/nm Lamp current/mA Passband width/nm Observation height/mm Flame type 217.6 10 0.2 6.5 ～ 7.0 Air-acetylene flame, lean burn 9.2 Establishment of standard curve Pipette 0 ml, 0.50 ml, 1.00 ml, 2.00 ml, 4.00 ml, 8.00 ml, 10.0 ml of antimony standard use solution (6.8) In a 25 ml volumetric flask, dilute to the mark with a nitric acid solution (6.4) and shake well. The mass concentration of this standard series are 0 mg/L, 2.00 mg/L, 4.00 mg/L, 8.00 mg/L, 16.0 mg/L, 32.0 mg/L, 40.0 mg/L. According to the reference test Measurement conditions (9.1), measuring the absorbance in order from low concentration to high concentration, and taking the standard series mass concentration (mg/L) as the horizontal sitting Use the corresponding absorbance as the ordinate to establish a standard curve. 9.3 Sample measurement The measurement of the sample was performed under the same conditions as the establishment of the standard curve (9.2). If the measurement result exceeds the standard curve The line range should be determined after diluting the sample with nitric acid solution (6.4). 9.4 Blank test The blank sample was measured under the same conditions as the sample measurement (9.3). 10 Calculation and representation of results 10.1 Calculation of results The mass concentration (mg/L) of antimony in the sample is calculated according to formula (1).   101 ) (  (1) Where. ρ--mass concentration of soluble antimony or total antimony in the sample, mg/L; ρ1--mass concentration of soluble antimony or total antimony in the sample obtained from the standard curve, mg/L; ρ0--mass concentration of soluble antimony or total antimony in the blank sample obtained from the standard curve, mg/L; V1-constant volume of sample, ml; V--sampling volume, ml; D--sample dilution. 10.2 Results representation When the measurement result is less than 100 mg/L, one decimal place is retained; when the measurement result is 100 mg/L or more, Keep three significant digits. 11 Precision and accuracy 11.1 Precision Six laboratories carried out unified samples containing soluble antimony with concentrations of 4.00 mg/L, 16.0 mg/L and 32.0 mg/L Six repeated determinations were performed. the relative standard deviations in the laboratory ranged from 1.2% to 3.6%, 0.9% to 2.2%, and 0.3% to 2.9%; relative standard deviations among laboratories were 4.0%, 2.2%, and 2.0%, respectively; repeatability limits were 0.3 mg/L and 0.6 mg/L, respectively And 0.7 mg/L; the reproducibility limits were 0.5 mg/L, 1.1 mg/L, and 2.0 mg/L, respectively. Six laboratories conducted microwave digestion of uniform industrial wastewater samples containing a total antimony mass concentration of 1.5 mg/L6 Repeated determination. the relative standard deviation in the laboratory ranges from 1.6% to 4.5%; the relative standard deviation between laboratories is 2.6%; The repeatability limit is 0.2 mg/L; the reproducibility limit is 0.2 mg/L. Six laboratories conducted a hot plate digestion method for a unified industrial wastewater sample with a total concentration of 1.5 mg/L of total antimony6 Repeated determination. The relative standard deviation in the laboratory ranges from 1.4% to 9.1%; the relative standard deviation between laboratories is 3.5% The repeatability limit is 0.2 mg/L; the reproducibility limit is 0.3 mg/L. 11.2 Accuracy Six laboratories performed six retests of certified standard samples (204906) with a mass concentration of (1.52 ± 0.05) antimony Repeat determination. The relative error range is -2.6% ~ 0.7%; the final relative error value is -0.8% ± 2.2%. Six laboratories used a unified domestic sewage sample with a total concentration of antimony that was not detected and a spiked concentration of 1.60 mg/L The microwave digestion method was used for 6 repeated spiking analysis. The recovery rate of spiking ranged from 87.7% to 104%. The final value is 97.0% ± 11.2%. Six laboratories for uniform industrial wastewater samples with a total antimony mass concentration of 1.5 mg/L and a spiked concentration of 2.00 mg/L Six repeated spiking analyses were performed with the microwave digestion method. the spiking recovery range was 86.7% to 105%; spiking recovery The final value of the rate is 97.8% ± 12.4%. Six laboratories for uniform industrial wastewater samples with a total antimony mass concentration of 1.5 mg/L and a spiked concentration of 2.00 mg/L Six repeated spiking analyses were performed using the hot-plate digestion method. The recovery range for spiking was 93.7% to 101%; The final yield was 97.4% ± 5.6%. 12 Quality Assurance and Quality Control 12.1 At least two laboratory blank samples shall be determined for each batch of samples, and the measurement results shall be lower than the detection limit of the method. 12.2 A standard curve should be established for each analysis sample, and the correlation coefficient should be ≥0.999. 12.3 Every 20 samples or each batch (≤20 samples/batch) should be analyzed at the middle concentration point of a standard curve. The relative error between the measurement result and the concentration at this point should be within ± 10%. 12.4 Every 20 samples or each batch (≤20 samples/batch) should be measured at least one parallel sample, the relative deviation of the measurement results Should be ≤20%. 12.5 Every 20 samples or each batch (≤20 samples/batch) should measure at least one matrix spiked sample, and the spiked recovery rate It should be controlled between 85% and 110%, or use a certified standard solution to control the accuracy of the measurement. 13 Waste treatment The waste liquid generated in the experiment should be collected separately, stored in a centralized manner, and properly labeled, and entrusted to a qualified unit for processing Management.

Appendix A

(Normative appendix) Matrix interference inspection method This method is suitable for samples with a certain concentration. Take two samples of the same sample, one of which is diluted 5 times (1 4), after dilution The measured value of the sample (not less than 10 times the detection limit) multiplied by the dilution factor is compared with the measured value of the undiluted sample. Differences within ± 10% are considered non-interfering. Otherwise, it indicates that interference exists and can be offset by dilution or standard addition method. When the diluted sample is less than 10 times the detection limit, the slope of the standard addition method curve can be compared with the slope of the standard curve. Relative deviations within ± 3% are considered non-interfering. Otherwise, matrix interference is present.

Appendix B

(Normative appendix) Standard addition method B.1 Establishment of calibration curve Add equal amounts of test samples to a blank of the same volume and three standard series of known different concentrations, assuming The concentration of the sample is Cx, the minimum concentration of the added standard is C0, C0≈0.5Cx, and the concentrations of the four samples are. Cx, Cx C0, Cx 2C0, Cx 3C0. Measure the absorbance of four samples, take the mass concentration of the standard solution as the abscissa, and use the The corresponding absorbance value is the ordinate. A standard curve is established. The intersection of the curve's reverse extension and the concentration axis is the quality of the sample to be tested. concentration. The relationship between the mass concentration of the sample to be tested and the standard curve of the standard addition method is shown in Figure B.1. Figure B.1 Relationship between the concentration of the sample to be tested and the standard curve of the standard addition method B.2 Precautions B.2.1 This method is only applicable to areas where the concentration of the sample to be measured is linear with the absorbance. B.2.2 The volume error caused by adding the standard solution should not exceed 0.5%. B.2.3 This method can only offset the effects caused by the matrix effect, not the effects of background absorption. Background absorption available deuterium The lamp method and the like perform background correction. B.2.4 The interference effect does not change with the concentration ratio of the element to be measured. Added standards and test elements The selected analytical conditions should have the same analytical response.

Appendix C

(Informative appendix) Applicability judgment of standard addition method Determine the absorbance of the sample to be tested as A, and check the mass concentration from the standard curve as x. Adding standards to the test sample Solution, the spiked concentration is s, the measured absorbance is B, and the concentration is y from the standard curve. Calculate the waiting time according to formula (C.1) Test sample content c. xy c    (C.1) When there is no matrix effect, s/(yx) should be 1, that is, c = x. At this time, the standard solution standard curve method can be used. When the basis For the body effect, s/(yx) is between 0.5 and 1.5, and the standard addition method can be used. If s/(yx) exceeds the range of 0.5 to 1.5, the standard addition method can be used. Not applicable. The matrix must be separated before measurement. ......

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