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HJ 749-2015 English PDF

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HJ 749-2015: Solid Waste. Determination of total chromium. Flame atomic absorption spectrometry
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Basic data

Standard ID HJ 749-2015 (HJ749-2015)
Description (Translated English) Solid Waste. Determination of total chromium. Flame atomic absorption spectrometry
Sector / Industry Environmental Protection Industry Standard
Word Count Estimation 14,144
Date of Issue 2015-08-21
Date of Implementation 2015-10-01
Older Standard (superseded by this standard) GB/T 15555.6-1995
Quoted Standard HJ/T 20; HJ/T 298; HJ/T 299; HJ/T 300; HJ 491; HJ 557
Regulation (derived from) Ministry of Environment Announcement 2015 No.54
Issuing agency(ies) Ministry of Ecology and Environment
Summary This standard specifies the flame atomic solid waste and solid waste leaching solution total chromium absorption spectrophotometry. This standard applies to the determination of solid waste and solid waste leaching solution total chromium. Determination of solid waste, the amount of sample is 0.2g, set the volume when a volume of 50ml, this standard detection limit of 8mg/kg, detection limit of 30mg/kg. Determination of solid waste leachate, when volume volume 50ml, this standard detection limit of 0.03mg/L, detection limit of 0.12mg/L.

HJ 749-2015: Solid Waste. Determination of total chromium. Flame atomic absorption spectrometry


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Solid Waste.Determination of total chromium.Flame atomic absorption spectrometry National Environmental Protection Standard of the People 's Republic of China Replacing GB/T 15555.6-1995 Determination of total chromium in solid waste Flame Atomic Absorption Spectrophotometry Solid Waste-Determination of total chromium -Flame atomic absorption spectrometry 2015-08-21 release 2015-10-01 implementation Ministry of Environmental Protection release I directory Preface .ii

1 Scope of application

2 normative reference documents

3 Principle of the method

4 interference and elimination

5 reagents and materials 1 6 instruments and equipment 2 7 Sample 2

8 Analysis steps

The results are calculated and expressed 10 precision and accuracy 11 Quality assurance and quality control 12 Precautions 13 Waste treatment .7 Appendix A (Normative Appendix) Standard Addition Act 8 Appendix B (informative appendix) Applicability judgment of standard addition method 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 the Prevention and Control of Environmental Pollution by Solid Wastes, Protect the environment, protect human health, regulate the determination of total chromium in solid waste, the development of this standard. This standard specifies the determination of total chromium in solid waste and solid waste leachate by flame atomic absorption spectrophotometry. This standard is for the determination of solid waste by total chromium in direct inhalation flame atomic absorption spectrophotometry (GB/T 15555.6-1995). This standard was first published in.1995, the original standard drafting unit for the China Environmental Monitoring Station, this is the first repair Set. The main contents of this revision are as follows. - Increased total chromium content in solid waste; - specifies the detection limit of the method; - a microwave digestion pretreatment method for the addition of solid waste leachate; - refine the precision and accuracy; - increased quality assurance and quality control requirements; - Added caution clause; - Increased waste disposal requirements. Since the implementation of this standard, the original State Environmental Protection Administration in.1995 approved the release of national environmental protection standards "Determination of total chromium in solid waste Direct inhalation flame atomic absorption spectrophotometry" (GB/T 15555.6-1995). Appendix A of this standard is a normative appendix, Appendix B is an informative appendix. This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division. The main drafting unit of this standard. Harbin Environmental Monitoring Center Station. The standard verification unit. Heilongjiang Province Environmental Monitoring Center Station, Dalian Environmental Monitoring Center, Anshan City Environmental Monitoring Central Station, Changchun City Environmental Monitoring Center Station, Qiqihar City Environmental Monitoring Center Station and Daqing Environmental Monitoring Center Station. The Environmental Protection Department of this standard approves on August 21,.2015. This standard is implemented on October 1,.2015. This standard is explained by the Ministry of Environmental Protection. Determination of total chromium - Solid waste - Flame atomic absorption spectrophotometric method WARNING. Disassembly shall be carried out in a fume hood and shall be protected against contact with skin and clothing as required.

1 Scope of application

This standard specifies the determination of total chromium in solid waste and solid waste leachate by flame atomic absorption spectrophotometry. This standard is applicable to the determination of total chromium in solid waste and solid waste leachate. Determination of solid waste, the sample volume of 0.2 g, constant volume of 50 ml, the detection limit of 8 mg/kg, measured The limit is 30 mg/kg. Determination of solid waste leaching solution, constant volume of 50 ml, the detection limit of 0.03 mg/L, The lower limit of determination was 0.12 mg/L.

2 normative reference documents

The contents of this standard refer to the following documents or their terms. Any annotated file that does not specify the date, its valid version Applicable to this standard. Technical specification for SJ sample preparation for industrial solid waste Technical Specification for Hazardous Waste Identification HJ/T 299 Solid waste leaching toxicity leaching method sulfuric acid nitric acid method HJ/T 300 solid waste leaching toxicity leaching method acetic acid buffer solution method Determination of total chromium in soil - Flame atomic absorption spectrophotometric method HJ 557 Solid waste leaching toxicity leaching method Horizontal oscillation method

3 Principle of the method

Solid waste leachate or solid waste digested by acid directly into the flame atomic absorption spectrophotometer air - B In the alkene flame, the formed chromium ground atoms generate absorption at 357.9 nm or other resonant lines with an absorbance value of Mass concentration is proportional.

4 interference and elimination

4.1 More than 7% HCl, HClO4 on the determination of chromium have a positive interference; HNO3 and H3PO4 negative interference. In the air - The interference elements in the acetylene flame are in the order of Cu > Ba > Al > Mg > Ca, Na, Sr, Zn, Sn. And these disturbances are independent of the existence of chromium (Cr3, Cr2O72-). 4.2 Fe3 produces negative interference, but has a positive interference on Cr6; Mn, Ni only negative interference with Cr3, without interfering with Cr6 Of the determination. When the use of poorly combustible air - acetylene flame, Fe and Ni interference becomes smaller, but the sensitivity of chromium determination significantly decreased low. In the sample by adding 1% to 2% of ammonium chloride can eliminate Fe, Ni, Mn and other metal elements and HCl, HNO3 and other acids Class interference. Adding 1% potassium pyrophosphate also eliminates the interference of coexisting metal components.

5 reagents and materials

Unless otherwise stated, analytical analytical reagents in accordance with national standards are used for the analysis, and the experimental water is freshly prepared Deionized water or distilled water. 5.1 Potassium Dichromate (K2Cr2O7). Reference reagent. 5.2 Ammonium persulfate [(NH4) 2S2O8]. 25.3 Ammonium chloride (NH4Cl). 5.4 Potassium pyrophosphate (K2S2O7). 5.5 nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure. 5.6 hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure. 5.7 Hydrogen peroxide. ρ (H2O2) = 1.11 g/ml, excellent grade pure. 5.8 hydrofluoric acid. ρ (HF) = 1.18 g/ml, excellent grade pure. 5.9 ammonium persulfate solution. ω ((NH4) 2S2O8) = 5%, weighed 5.0 g ammonium persulfate (5.2) dissolved in 100 ml water in. 5.10 ammonium chloride solution. ω (NH4Cl) = 10%, weighed 10.0 g ammonium chloride (5.3) dissolved in 100 ml of water. 5.11 potassium pyrosulfate solution. ω (K2S2O7) = 1%, weighed 1.0 g potassium pyrophosphate (5.4) dissolved in 100 ml of water. 5.12 nitric acid solution. 1 99 (V/V), prepared with concentrated nitric acid (5.5). 5.13 nitric acid solution. 1 1 (V/V), with concentrated nitric acid (5.5) preparation. 5.14 hydrochloric acid solution. 1 2 (V/V), prepared with concentrated hydrochloric acid (5.6). 5.15 chromium standard stock solution. ρ (Cr) = 1000 mg/L Purchase a commercially available standard material/certified standard sample, or accurately weigh 0.2829 g of reference potassium dichromate (5.1), with A small amount of water dissolved, transferred to 100ml volumetric flask, the experimental water volume after shake, at room temperature for 6 months. 5.16 chromium standard use of liquid. ρ (Cr) = 50.0 mg/L Accurate amount of chromium standard stock solution (5.15) 5.00 ml in 100 ml volumetric flask, the experimental water volume shake. 5.17 Gas. acetylene, purity ≥99.0%. 5.18 Gas. Air, before entering the burner should be properly filtered to remove water, oil and other impurities.

6 instruments and equipment

6.1 flame atomic absorption spectrophotometer. 6.2 Chrome hollow cathode lamp. 6.3 air compressor, should be equipped with water, degreasing and dust removal device. 6.4 Microwave digestion. with temperature control and program temperature function, the temperature accuracy of up to ± 2 ℃. 6.5 Electric plate. with temperature control function. 6.6 balance. accuracy of 0.0001 g. 6.7 Balance. Accuracy 0.01 g. 6.8 Teflon crucible. 6.9 nylon screen. 100 mesh. 6.10 General laboratory equipment and equipment commonly used.

7 samples

7.1 Collection and storage of samples The collection and storage of solid waste samples are carried out in accordance with the relevant provisions of HJ/T 20 and HJ/T 298. 7.2 Preparation of the sample 7.2.1 Solid waste samples The preparation of solid waste samples was carried out in accordance with the relevant provisions of HJ/T 20. For solid waste or viscous sludge 3 items, accurately weighed 10 g samples (m1, accurate to 0.01 g), natural dry or freeze-dried, weighing again (m2, fine To 0.01 g), grinding, all over 100 mesh sieve. 7.2.2 Solid waste leachate samples A sample of solid waste leachate was prepared according to the method of HJ/T 299, HJ/T 300 and HJ 557. 7.3 Preparation of samples 7.3.1 Solid waste samples 7.3.1.1 Electric plate digestion method Weigh 0.2 g (m3, accurate to 0.0001 g) solid waste sample (7.2.1) in 50 ml polytetrafluoroethylene crucible, After wetting with water, add 10 ml of concentrated hydrochloric acid (5.6), in the fume hood on the hot plate at 50 ℃ heating, the initial decomposition of the sample, To be evaporated to about 3 ml or so, add 5 ml of concentrated nitric acid (5.5), 5 ml of hydrofluoric acid (5.8), stamped in the hot plate About 120 ~ 130 ℃ heating 0.5 ~ 1 h or so, open the lid by adding 2 ml of hydrogen peroxide (5.7), and then cover 150 ~ 160 ℃ Heating about 1 h, and then open the lid, drive white smoke and steamed into the contents of the liquid is not the state of the liquid beads (hot observation). can (5.5), 3 ml hydrofluoric acid (5.8), 1 ml hydrogen peroxide (5.7), repeat the addition of 3 ml of concentrated nitric acid (5.5) Above the digestion process. Remove the crucible slightly cold, add 1 ml of nitric acid solution (5.13), heat dissolve the soluble residue, Try to move to 50 ml volumetric flask, add 5 ml of ammonium chloride solution (5.10), the experimental water volume (Vo), to be tested. Note 1. 30% of the total amount of hydrogen peroxide can not exceed 10ml. 7.3.1.2 Microwave digestion method Weigh 0.2 g (m3, accurate to 0.0001 g) solid waste sample (7.2.1) in a microwave digestion tank with a small amount of water After wetting, 3 ml of concentrated nitric acid (5.5) and 1 ml of concentrated hydrochloric acid (5.6) were added and digested with reference to Table 1. After cooling, the contents All moved to 50 ml polytetrafluoroethylene crucible, stamped, placed in the hot plate, micro boiling state to drive white smoke, to white smoke is not And then 2 ml of experimental water, 3 ml of hydrofluoric acid (5.8) and 2 ml of hydrogen peroxide (5.7), followed by Continue heating, add 1 ml of hydrogen peroxide (5.7), to the reaction is stable, continuous heating to the contents of a viscous. Remove Slightly cool, add 3 ml of hydrochloric acid solution (5.14), dissolve the soluble residue in warm, the whole volume to 50 ml volumetric flask, add 5 ml ammonium chloride solution (5.10), experimental water volume (Vo), to be tested. Note 2. microwave digestion if the digestion has been clarified, then do not have to add hydrofluoric acid and hydrogen peroxide, acid directly after the constant volume. Table 1 microwave digestion instrument reference conditions Program temperature rise time (min) Decomposition temperature holding time (min) The first step 10 room temperature ~ 170 ℃ 5 The second step 10 170 ℃ ~ 175 ℃ 5 7.3.2 Solid waste leachate sample (1) electric plate digestion method Measure the amount of 50.00 ml (V2) leachate (7.2.2) in a 150 ml Erlenmeyer flask, add 2 ml of concentrated nitric acid (5.5) And 5 ml of ammonium persulfate solution (5.9), shake. In the triangle bottle into the small funnel placed on the hot plate after heating, boiling to When the volume of the test solution is about 20 ml, it is removed and cooled. If the test solution is viscous, should add 2 ml of concentrated nitric acid (5.5), continue to heat, repeat the above operation, to test solution to clarify Or the color remains the same. Rinse the small funnel and the inner wall of the flask with a small amount of test water and move all the test solution to 50 ml Volume flask, add 5 ml ammonium chloride solution (5.10), experimental water volume (V1), to be tested. 4 (2) Microwave digestion method Measure the amount of 5.00 to 10.00 ml leachate (7.2.2) in a microwave digestion tank, add 1 ml of concentrated nitric acid (5.5) and 1 ml ammonium persulfate solution (5.9), digestion with reference to Table 1, after cooling the solution to 50 ml volumetric flask, with less The amount of experimental water rinse the microwave digestion tank, the test solution all moved to 50 ml volumetric flask, add 5 ml of ammonium chloride solution (5.10), experimental water volume (V1), to be measured. Note 3. microwave digestion method is not suitable for digestion of high organic content of the sample, such as leaching solution contains high organic matter, the proposed use of electricity Hot plate method. 7.4 Preparation of blank sample 7.4.1 Solid waste blank sample The solid waste blank sample was prepared according to the procedure of 7.3.1.1. 7.4.2 Solid waste leachate blank sample The solid waste leachate blank sample was prepared according to 7.3.2.1.

8 Analysis steps

8.1 Instrument reference conditions Different models of atomic absorption spectrophotometer the best working conditions are different, should be in accordance with the instructions to operate the instrument, The recommended conditions for this instrument are as follows. Table 2 Reference measurement conditions Element Cr Determination of wavelength (nm) 357.9 Passband width (nm) 0.7 Flame nature Flammable flame Sub-sensitive line (nm) 359.0; 360.5; 425.4 Burner height (mm) so that the hollow cathode lamp spot through the bright blue part Note 4. After igniting the acetylene-air flames, the burner temperature should be allowed to reach the thermal equilibrium before being measured. 8.2 Calibration Respectively, the amount of 0,0.50,1.00,2.00,3.00,5.00 ml chromium standard use of liquid (5.16) in the 50 ml volumetric flask , Add 5 ml of ammonium chloride solution (5.10), with nitric acid solution (5.12) constant volume to the mark, mix. This standard Series concentrations were. 0,0.50,1.00,2.00,3.00,5.00 mg/L. The absorbance of the standard series was measured in turn from low to high concentrations according to the reference measurement conditions (8.1). To zero concentration Correct the absorbance as the ordinate and plot the calibration curve with the concentration of chromium (mg/L) as the abscissa. Note 5. When the sample matrix composition is complex or unknown, or spike recovery rate of more than the scope of the requirements of this method should be used standard The results are shown in Appendix A, and the applicability of the standard addition method is given in Appendix B. 8.3 Sample determination The prepared sample was measured with the same instrumental analysis conditions as the calibration curve. When the sample concentration exceeds the calibration curve The maximum concentration of the sample can reduce the amount of sample or increase the dilution factor. 8.4 blank test 5 Prepare the prepared blank sample 7.4 according to the instrument reference conditions (8.1).

9 Results calculation and representation

9.1 Calculation of solid waste test results 9.1.1 Solid and viscous sludge solid waste The total chromium content in solid waste  (mg/kg) is calculated according to equation (1). V  00) ( (1) Where.  - total chromium content in solid waste, mg/kg;  - the concentration of total chromium in the sample taken from the calibration curve, mg/L; 0 - Concentration of total chromium in blank samples taken on the calibration curve, mg/L; V0 - volume after digestion, ml; M1 - the quality of solid samples, g; M2 - the quality of the solid sample after drying, g; M3 - the quality of the sample after grinding, g; F - dilution factor. 9.1.2 Liquid and semi-solid (except viscous sludge) Solid waste The total chromium content in solid waste  (mg/kg) is calculated according to formula (2). V  00) ( (2) Where.  - total chromium content in solid waste, mg/kg;  - the concentration of total chromium in the sample taken from the calibration curve, mg/L; 0 - Concentration of total chromium in blank samples taken on the calibration curve, mg/L; V0 - volume after digestion, ml; M3 - the quality of the sample, g; F - dilution factor. 9.2 Calculation of solid waste leachate test results The concentration of total chromium in the solid waste leachate is calculated (in mg/L) according to equation (3). V  101) ( (3) Where.  - concentration of total chromium in the solid waste leachate, mg/L; 1 ü - the concentration of total chromium in the sample taken from the calibration curve, mg/L; 0 - Concentration of total chromium in blank samples taken on the calibration curve, mg/L; V1 - volume of decoction after decoction, ml; 6V2 - when the volume of leaching solution, ml; F - dilution factor. 9.3 The result is shown When the solid waste sample determination results less than 100 mg/kg, retained to the integer position; when the determination is greater than or equal to 100 Mg/kg, retain 3 valid digits. When the solid waste leachate sample determination results less than 1 mg/L, the retention of two decimal places; when the determination is greater than Equal to 1 mg/L, retain 3 valid digits. 10 precision and accuracy 10.1 Precision For solid waste, six laboratories were treated with sewage at a concentration of 135.5 mg/kg and 125.0 mg/kg, respectively Plant sludge samples, industrial sludge samples and zinc slag standard samples were measured, the relative standard deviation of the laboratory were 6.0% ~ 11.5%, 5.4% ~ 12.7%, 3.6% ~ 7.4%, the relative standard deviation between the laboratory were 4.9%, 6.0% 4.2%, repeatability r were 78 mg/kg, 68 mg/kg, 17 μg/g, reproducibility R were 389 mg/kg, 356 Mg/kg, 128 μg/g. For solid waste leachate, six laboratories had a total chromium mass concentration of 0.25 mg/L, 1.20 mg/L and 2.20 Mg/L leaching solution samples were measured, the relative standard deviation in the laboratory 0.2 ~ 3.0%, 0.2 ~ 3.3%, 0.2 ~ 1.6%; the relative standard deviations were 1.7%, 4.3%, 5.5%, respectively. The repeatability r was 0.02 mg/L, 0.10 mg/L And 0.07 mg/L; reproducibility R was 0.02 mg/L, 0.17 mg/L and 0.35 mg/L. 10.2 Accuracy For solid waste, six validation laboratories measured the zinc residue reference material with a relative error of 0.45 to 8.6% The final error is 4.4% ± 5.2%. For solid waste leachate, six laboratories had a total chromium mass concentration of 0.25 mg/L and 1.20 mg/L The recoveries were as follows. 95.0 ~ 117% and 95.0 ~ 106%, respectively. The final values were 103% ± 15.0% and 99.4% ± 8.0%. 11 quality assurance and quality control 11.1 Each batch of samples should be blank test, the determination results should be lower than the method detection limit. Each sample of 20 samples should be carried out one Analysis of zero - concentration samples. If the determination result is higher than the method detection limit, calibration curve zero, re-determination of the sample. 11.2 The calibration curve shall be plotted for each sample analysis and the correlation coefficient should be greater than or equal to 0.999. 11.3 Each 20 samples should be analyzed for a calibration curve of the intermediate point concentration standard solution, the measurement results with the calibration curve for the The relative deviation of the point concentration should be less than or equal to 10%. Otherwise, the calibration curve needs to be redrawn. 11.4 each batch of samples should be at least 10% of the parallel sample determination (the number of samples less than 10 at least one), two parallel The relative deviation of the sample analysis results should be less than 20%. 11.5 each batch of samples should be at least 10% spike recovery sample test (the number of samples less than 10 at least one), plus standard Yield should be between 85 ~ 120%. 12 Precautions 12.1 Glass containers used in the experiment were first soaked with 10% nitric acid solution for 24 h, then rinsed with tap water and experimental water Clean, dry in a clean environment. The entire cleaning process shall not use potassium dichromate lotion. 712.2 Burner height has a significant effect on the sensitivity of chromium. The burner height should be adjusted to the optimum. At this time not only measured High sensitivity, stable reading, and less interference. 12.3 Determination of chromium wavelength is more sensitive to 357.9 nm line, can determine the low content of chromium. 359.4,360.5 nm Line sensitivity is slightly lower than 357.9 nm line, can also be used. However, when measuring high levels of chromium, it is recommended to use 425.5 nm, 427.5 Nm or 429.0 nm lines. They are in the visible region, subject to molecular absorption and other spectral interference is small, the sensitivity than 357.9 nm Low 3 to 5 times. 12.4 If the liquid after solidification of ac...

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