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Basic dataStandard ID: HJ 1193-2021 (HJ1193-2021)Description (Translated English): (Water quality Determination of indium Graphite furnace atomic absorption spectrophotometry) Sector / Industry: Environmental Protection Industry Standard Word Count Estimation: 11,137 Issuing agency(ies): Ministry of Ecology and Environment HJ 1193-2021: (Water quality Determination of indium Graphite furnace atomic absorption spectrophotometry)---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. (Water quality Determination of indium Graphite furnace atomic absorption spectrophotometry) National Ecological Environment Standard of the People's Republic of China Determination of Indium in Water Quality graphite furnace atomic absorption spectrophotometry Water quality-Determination of indium -Graphite furnace atomic absorption spectrometry This electronic version is the official standard text, which is reviewed and typeset by the Environmental Standards Institute of the Ministry of Ecology and Environment. Posted on 2021-09-17 2022-01-01 Implementation Released by the Ministry of Ecology and Environment directory Foreword...ii 1 Scope...1 2 Normative references...1 3 Terms and Definitions...1 4 Principles of the method...1 5 Interference and cancellation...1 6 Reagents and materials...2 7 Instruments and equipment...2 8 Samples...3 9 Analysis steps...3 10 Result calculation and representation...4 11 Accuracy...5 12 Quality Assurance and Quality Control...5 13 Waste Disposal...5 14 Notes...5 Appendix A (Informative Appendix) Standard Addition...6 Appendix B (Informative Appendix) Microwave Digestion...8 Determination of Indium in Water Quality by Graphite Furnace Atomic Absorption Spectrophotometry Warning. Nitric acid is highly corrosive and oxidizing, the sample pretreatment process should be carried out in a fume hood, and protective clothing should be worn as required during operation Protective equipment and avoid contact with skin and clothing. 1 Scope of applicationThis standard specifies the graphite furnace atomic absorption spectrophotometry for the determination of indium in water. This standard applies to the determination of indium in surface water, groundwater and industrial wastewater. When the injection volume was 20 μl, the detection limit of the method was 2 μg/L, and the lower limit of determination was 8 μg/L.2 Normative referencesThis standard refers to the following documents or clauses thereof. For dated references, only the dated version applies to this standard. For undated references, the latest edition (including all amendments) applies to this standard. HJ/T 91 Technical Specification for Surface Water and Sewage Monitoring HJ 91.1 Technical Specification for Wastewater Monitoring HJ 164 Technical Specification for Groundwater Environmental Monitoring HJ 677 Digestion of Total Metals in Water Quality Nitric Acid Digestion Method HJ 678 Microwave digestion method for the digestion of total metals in water quality3 Terms and DefinitionsThe following terms and definitions apply to this standard. 3.1 soluble indium Determination of indium in unacidified samples after filtration through a 0.45 μm filter. 3.2 total indium quantity of indium Determination of indium after digestion of unfiltered samples.4 Principles of the methodAfter the sample is filtered or digested, it is injected into the graphite furnace atomizer, and after drying, ashing and atomization, the indium ground state atomic vapor is formed. The characteristic spectral line emitted by the heart cathode lamp or other light source produces selective absorption, and its absorbance is proportional to the concentration of indium within a certain range.5 Interference and cancellation5.1 Ag, Al, As, B, Ba, Be, Bi, Cd, Co, Cr, Cu, Mn, Mo, Ni, Determination of Pb, Se, Sr, Ti, Tl, V, Zn, K, Na, Mg, Ca, Fe below 500 mg/L and Cl-pair below 10000 mg/L Results were not significantly affected. 5.2 When the interference of the sample matrix is serious, the standard addition method can be used for determination, see Appendix A.6 Reagents and MaterialsUnless otherwise specified, analytical reagents that meet national standards are used in the analysis, and the experimental water is distilled or deionized water. 6.1 Nitric acid (HNO3). ρ=1.42 g/ml. 6.2 Palladium nitrate [Pd(NO3)2·2H2O]. 6.3 Magnesium nitrate [Mg(NO3)2·6H2O]. excellent grade. 6.4 Indium. Spectroscopically pure. 6.5 Nitric acid solution. φ=50%. Nitric acid (6.1) and water are mixed in a volume ratio of 1.1. 6.6 Nitric acid solution. φ=1%. Nitric acid (6.1) and water are mixed in a volume ratio of 1.99. 6.7 Matrix modifier. mixed solution of palladium nitrate-magnesium nitrate. Weigh 0.26 g of palladium nitrate (6.2), add 2 ml of nitric acid (6.1) and dissolve in a small amount of water. Weigh 0.11 g of magnesium nitrate (6.3), use a small amount of Water dissolves. Mix the 2 solutions and make up to 100 ml with water. 6.8 Indium standard stock solution. ρ(In)=100 mg/L. Accurately weigh 0.1 g (accurate to 0.0001 g) indium (6.4), add 50 ml of nitric acid solution (6.5), heat to dissolve completely, after cooling Transfer to a 1000 ml volumetric flask, make up to the mark with water, and shake well. Transfer to a polyethylene bottle and seal for 2 years. Commercially available Certified standard solution. 6.9 Indium standard intermediate solution. ρ(In)=10.0 mg/L. Pipette 10.00 ml of indium standard stock solution (6.8) into a 100 ml volumetric flask, dilute to the mark with nitric acid solution (6.6), and shake well. change Sealed in polyethylene bottles, it can be stored for 6 months. 6.10 Indium standard solution. ρ(In)=500 μg/L. Pipette 5.00 ml of indium standard intermediate solution (6.9) into a 100 ml volumetric flask, dilute to the mark with nitric acid solution (6.6), and shake well. change Sealed in polyethylene bottles, it can be stored for 1 month. 6.11 Argon. purity ≥99.99%. 6.12 Membrane. Aqueous microporous membranes such as cellulose acetate and polyethylene with a pore size of 0.45 μm.7 Instruments and equipment7.1 Sample bottle. 500 ml, polyethylene or equivalent. 7.2 Graphite furnace atomic absorption spectrophotometer. with background correction function. 7.3 Indium hollow cathode lamps or other light sources. 7.4 Temperature control electric heating plate. with temperature control function. 7.5 Common laboratory instruments and equipment.8 samples8.1 Collection of samples In accordance with the relevant provisions of HJ/T 91, HJ 91.1 and HJ 164, samples for the determination of soluble indium and total indium should be collected separately. 8.2 Storage of samples 8.2.1 Soluble Indium After the sample is collected, filter it with a water-based microporous membrane (6.12), discard the initial filtrate, and collect the required volume of filtrate in the sample bottle (7.1). Add 1 ml of nitric acid (6.1) per 100 ml of filtrate to acidify, and measure within 1 month. 8.2.2 Total Indium After sample collection, acidify with 1 ml of nitric acid (6.1) per 100 ml of sample, store in vials (7.1), and measure within 1 month. 8.3 Preparation of test specimens 8.3.1 Soluble Indium See 8.2.1 for sample processing methods. 8.3.2 Total Indium Measure 50.0 ml of the well-mixed water sample (8.2.2) into a 150 ml glass beaker, add 5 ml of nitric acid (6.1), and place it in a temperature-controlled electric heating On the plate (7.4), cover with a watch glass to keep it in a slightly boiling state. When the sample is uniform and clear, remove the watch glass and evaporate to about 5 ml. cold After cooling, rinse the inner wall of the beaker and the watch glass at least 3 times with water, transfer the whole amount into a 50 ml volumetric flask, make up to the mark with water, and shake well for measurement. Note 1.The volume of nitric acid added can be adjusted according to actual needs. Note 2.The hot plate digestion of the sample can also be carried out in accordance with HJ 677.For the microwave digestion method of the sample, see Appendix B. 8.4 Preparation of blank samples Substitute the same batch of experimental water for the sample, and prepare the blank sample according to the same steps as the sample preparation (8.3).9 Analysis steps9.1 Reference measurement conditions Adjust the instrument to the best working state according to the instrument instruction manual, see Table 1 for reference measurement conditions, and see Table 2 for the recommended heating program of the graphite furnace. Table 1 Reference measurement conditions Light source wavelength (nm) Lamp current (mA) Passband width (nm) Injection volume (μl) Indium Hollow Cathode Lamp 325.6 15 0.7 20 Note. The wavelength of 303.9 nm can also be used for measurement. 9.2 Plotting the standard curve Pipette 0.00 ml, 0.50 ml, 1.00 ml, 2.00 ml, 3.00 ml, 5.00 ml of indium standard solution (6.10) to 50 ml respectively In a volumetric flask, make up to the mark with nitric acid solution (6.6) and shake well. The concentration of standard series is 0.00 μg/L, 5.00 μg/L, 10.0 μg/L, 20.0 μg/L, 30.0 μg/L, 50.0 μg/L. According to the reference measurement conditions (9.1), add to the graphite tube sequentially from low concentration to high concentration 20 μl standard solution and 5 μl matrix modifier (6.7), measure the absorbance. Taking the indium concentration as the abscissa and the absorbance as the ordinate, draw the standard Quasi curve. 9.3 Determination of samples Measure the prepared sample (8.3) according to the same measurement conditions (9.1) and operating steps (9.2) as for drawing the standard curve. If the measurement result exceeds the standard curve range, the sample should be diluted with nitric acid solution (6.6) and re-measured. 9.4 Blank test Carry out the prepared blank sample (8.4) according to the same measurement conditions (9.1) and operation steps (9.2) as for drawing the standard curve Determination. 10 Result calculation and presentation 10.1 Result calculation The concentration of indium in the sample (μg/L) is calculated according to formula (1). ρ=ρ1×D (1) In the formula. ρ--the concentration of indium in the sample, μg/L; ρ1--The concentration of indium in the sample obtained from the standard curve, μg/L; D--dilution factor of the sample. 10.2 Result representation When the measurement result is less than 100 μg/L, it is reserved to the integer; when the measurement result is greater than or equal to 100 μg/L, 3 valid digits are reserved. number. 11 Accuracy 11.1 Precision Surface water with an average concentration of 6 μg/L of soluble indium and groundwater with an average concentration of 20 μg/L were spiked by six laboratories Six repeated determinations were performed. the relative standard deviations within the laboratory were 7.3% to 14% and 3.4% to 7.4%; the relative standard deviations between the laboratories were The differences were 9.5% and 4.4%, respectively; the repeatability limits were 2 μg/L and 4 μg/L, respectively; the reproducibility limits were 3 μg/L and 4 μg/L, respectively. 6 laboratories respectively unified the actual samples of 3 kinds of total indium with the average measured concentration of 10 μg/L, 16 μg/L and 23 μg/L of industrial wastewater. Six repeated determinations were performed. the relative standard deviations within the laboratory were 6.7%-13%, 4.3%-7.4%, and 2.8%-5.8%; The relative standard deviations were 7.7%, 5.9%, and 4.6%, respectively; the repeatability limits were 3 μg/L, 3 μg/L, and 4 μg/L, respectively; the reproducibility limits were 4 μg/L, 4 μg/L, and 4 μg/L, respectively. 4 μg/L, 5 μg/L. 11.2 Correctness The average measured concentrations of 2 kinds of 6 laboratories were lower than the detection limit of the method, and the spiked concentration was 7 μg/L surface water and 8 μg/L The unified real samples of groundwater were analyzed and determined by repeated standard addition for 6 times. the standard addition recoveries were 96.7%-115% and 86.5%-106%, respectively; The final recovery of standard addition was 102%±16.6% and 96.1%±14.2%, respectively. The 6 laboratories respectively measured the average concentrations of 3 kinds of 10 μg/L, 16 μg/L, 23 μg/L, and the spiked concentrations were 7 μg/L, 15 μg/L, The 20 μg/L industrial wastewater unified actual sample was subjected to 6 repeated standard addition analysis and determination. the standard addition recoveries were 97.4%-119%, 79.6%～101%, 87.3%～107%; the final recovery of standard addition was 107%±15.0%, 91.6%±17.0%, 97.0%±16.2%, respectively. 12 Quality Assurance and Quality Control 12.1 At least one blank sample should be determined for each batch of samples, and the determination result should be lower than the detection limit of the method. 12.2 A standard curve should be drawn for each batch of sample analysis. The standard curve should contain at least 6 concentration points (including zero point), and the correlation coefficient of the standard curve Should not be less than 0.995.The middle concentration point of the standard curve should be checked for every 10 samples measured, and the relative error of the measurement results should be within ±10% within. Otherwise, the standard curve should be redrawn. 12.3 At least 10% of the parallel double samples shall be measured for each batch of samples. When the number of samples is less than 10, at least one parallel double sample shall be measured. parallel double The relative deviation of the sample determination should be within ±20%. 12.4 At least 10% of the matrix spiked samples should be measured for each batch of samples. When the number of samples is less than 10, at least one matrix spiked sample should be measured. The recovery of standard addition should be between 70% and 130%. 13 Waste Disposal The waste liquid generated in the experiment should be placed in a closed container for classified collection, centralized storage, and entrusted to a qualified unit for treatment according to law. 14 Notes 14.1 After the measurement of high concentration samples or when the blank value is high, increase the number of times of empty burning of the graphite tube to eliminate the memory effect. 14.2 When using metal indium to prepare standard stock solution, it is necessary to first remove the contaminants on the surface with polishing sandpaper above 1000, and then use anhydrous ethyl acetate. Rinse with alcohol.Appendix A(informative appendix) standard accession A.1 Calibration curve drawing method Measure 4 equal parts of the sample to be tested (concentration is ρ), and prepare 4 solutions with the same total volume. 1 without standard solution, the remaining 3 The standard solutions of different concentrations are added in proportion to each other, and the solution concentrations are usually. ρ, ρ+ρ0, ρ+2ρ0, ρ+3ρ0; adding standard solution The concentration of the liquid ρ0 is approximately equal to 0.5 times the concentration of the sample, ie ρ0 ≈ 0.5ρ. Use blank solution to zero, measure the absorbance of 4 solutions in turn under the same conditions, take the concentration of added standard solution as the abscissa, absorb The luminosity is the ordinate, and the calibration curve is drawn. The intersection of the reverse extension of the curve and the abscissa is the concentration of the sample to be tested. The concentration of the sample to be tested is The relationship between the absorbance should be shown in Figure A.1. A.2 Precautions A.2.1 This method is only applicable to the region where the concentration of the sample to be tested is linear with the absorbance. A.2.2 The volume error caused by adding the standard solution should not exceed 0.5%. A.2.3 This method can only compensate for the influence caused by the matrix effect, but cannot compensate for the influence of background absorption. A.3 Applicability judgment of standard addition method The concentration ρ of indium in the sample is calculated according to formula (A.1). ρ = ρ3/(ρ2-ρ1)×ρ1 (A.1) In the formula. ρ--the concentration of indium in the sample, μg/L; ρ3--concentration of indium standard solution added to the sample to be tested, μg/L; ρ2--The concentration of indium in the test sample with the added concentration of ρ3 obtained from the standard curve, μg/L; ρ1--The concentration of indium in the sample obtained from the standard curve, μg/L. When the matrix effect exists, ρ3/(ρ2-ρ1) is between 0.5 and 1.5, and the standard addition method can be used; when ρ3/(ρ2-ρ1) exceeds this range, the standard addition method can be used. Accession laws do not apply.Appendix B(informative appendix) microwave digestion B.1 Preparation of samples Measure 25.0 ml of the well-mixed water sample (8.2.2) into a microwave digestion tank, add 2 ml of nitric acid (6.1), leave it for 30 minutes, and cover it Sealed, placed in a microwave digestion apparatus, 10 min from room temperature to 180 °C and maintained for 15 min. After the digestion is completed, cool to room temperature, and the digestion The pot is placed on an electric hot plate and heated and evaporated to about 5 ml in a near-boiling state. After cooling, rinse the inner wall and lid of the digestion vessel with water at least 3 times, Transfer the whole amount into a 25 ml volumetric flask, make up to the mark with water, and shake well for measurement. Note. 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