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GB/T 38596-2020 English PDF

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GB/T 38596-2020: Determination method of heavy metal contents in the wastewater during catalyst production
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PDF similar to GB/T 38596-2020


Standard similar to GB/T 38596-2020

GB/T 37355   GB/T 37354   GB/T 37359   GB/T 38691   GB/T 38602   

Basic data

Standard ID GB/T 38596-2020 (GB/T38596-2020)
Description (Translated English) Determination method of heavy metal contents in the wastewater during catalyst production
Sector / Industry National Standard (Recommended)
Classification of Chinese Standard G74
Classification of International Standard 71.100.99
Word Count Estimation 6,692
Date of Issue 2020-03-31
Date of Implementation 2021-02-01
Quoted Standard GB/T 602; GB/T 603; GB/T 6682
Issuing agency(ies) State Administration for Market Regulation, China National Standardization Administration
Summary This standard specifies the method for the determination of heavy metal content in catalyst production wastewater. This standard applies to the determination of the total amount and dissolved content of copper (Cu), lead (Pb), bismuth (Bi), antimony (Sb), cobalt (Co), and nickel (Ni) in catalyst production wastewater.

GB/T 38596-2020: Determination method of heavy metal contents in the wastewater during catalyst production


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Determination method of heavy metal contents in the wastewater during catalyst production ICS 71.100.99 G74 National Standards of People's Republic of China Determination of heavy metal content in catalyst production wastewater 2020-03-31 released 2021-02-01 implementation State Administration for Market Regulation Issued by the National Standardization Management Committee

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard was proposed by the China Petroleum and Chemical Industry Federation. This standard is under the jurisdiction of the National Chemical Standardization Technical Committee (SAC/TC63). Drafting organizations of this standard. Nanjing Huiwen New Material Technology Development Co., Ltd., Shandong Product Quality Inspection and Research Institute, Shandong Qingbo Ecological Materials Comprehensive Utilization Co., Ltd., Haohua Chemical Technology Group Co., Ltd., Sinopec Nanjing Chemical Research Institute Co., Ltd., Dongguan Wei Side Science and Technology Development Co., Ltd., Yancheng Metrology and Testing Institute. The main drafters of this standard. Zou Huiling, Qiu Ailing, Xia Pandeng, He Chengguo, Jiang Tiankai, Shi Tianbao, Zhao Wei, Xie Yingqiang, Zhang Wenfu, Tan Ge. Determination of heavy metal content in catalyst production wastewater Warning --- Some reagents used in this standard are toxic or corrosive, and some operations are dangerous. This standard does not disclose There may be safety issues, users should be careful and responsible for taking appropriate safety and health measures when operating.

1 Scope

This standard specifies the determination method of heavy metal content in catalyst production wastewater. This standard applies to the total amount and dissolution of copper (Cu), lead (Pb), bismuth (Bi), antimony (Sb), cobalt (Co), and nickel (Ni) in catalyst production wastewater Determination of state content.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article Pieces. For undated references, the latest version (including all amendments) applies to this document. GB/T 602 Preparation of standard solutions for impurity determination of chemical reagents Preparation of preparations and products used in GB/T 603 chemical reagent test method GB/T 6682 Analytical laboratory water specifications and test methods

3 General rules

When there are no other requirements for the reagents used in this standard, inductively coupled plasma emission spectroscopy uses superior grade pure reagents, flame atoms Absorption spectroscopy uses analytical reagents; when no other requirements are specified, the water used refers to the secondary water specified in GB/T 6682.Testing The standard solutions, preparations and products used for impurity determination are in accordance with the regulations of GB/T 602 and GB/T 603 unless other requirements are specified. Order preparation.

4 Reagents or materials

4.1 Nitric acid. 4.2 Perchloric acid. 4.3 Nitric acid solution. 11. 4.4 Nitric acid solution. 99. 4.5 Copper standard solution. 1g/L. Weigh 1g (accurate to 0.0001g) of metallic copper (spectral purity), and heat it with 30mL nitric acid solution (4.3) to dissolve it. After cooling, make the volume to 1L with water. 4.6 Lead standard solution. 1g/L. Weigh 1g (accurate to 0.0001g) of metallic lead (spectral purity), and heat it with 30mL nitric acid solution (4.3) to dissolve it. After cooling, make the volume to 1L with water. 4.7 Bismuth standard solution. 1g/L. Weigh 1g (accurate to 0.0001g) of metallic bismuth (spectral purity), and use 50mL of nitric acid solution (4.3) to heat it to dissolve After dissolving completely, cool to room temperature and dilute to 1L with water. 4.8 Antimony standard solution. 1g/L. Weigh 1g (accurate to 0.0001g) metal antimony (spectral purity), and use 20mL~30mL sulfuric acid solution (1 1) Heat to dissolve, and dilute to 1L with sulfuric acid solution (1 4). 4.9 Cobalt standard solution. 1g/L. Weigh 1g (accurate to 0.0001g) of metallic cobalt (spectrally pure), and use 50mL of nitric acid solution (4.3) to heat to dissolve After cooling, make the volume to 1L with water. 4.10 Nickel standard solution. 1g/L. Weigh 1g (accurate to 0.0001g) of metallic nickel (spectral purity) and heat it with 30mL nitric acid solution (4.3) Dissolve and dilute to 1L with water after cooling. 4.11 Copper, lead, bismuth, antimony, cobalt, and nickel mixed standard solutions. copper, lead, bismuth, antimony, cobalt, and nickel are all 100 mg/L. Measure 10.00mL copper separately Standard solution (4.5), lead standard solution (4.6), bismuth standard solution (4.7), antimony standard solution (4.8), cobalt standard solution (4.9), nickel standard solution (4.10) Placed in a 100mL volumetric flask, add 4mL of nitric acid solution (4.3), dilute to 100mL with water, and shake well. 4.12 Copper, lead, and nickel mixed standard solution. copper, lead, and nickel are all 100mg/L. Measure 10.00mL copper standard solution as needed (4.5) One or more of lead standard solution (4.6) and nickel standard solution (4.10) are placed in a 100mL volumetric flask, and 5mL nitric acid solution is added (4.3), dilute to 100mL with water, shake well.

5 samples

5.1 Collect samples with polyethylene bottles. The sampling bottle is first washed with detergent, then soaked in nitric acid solution (4.3), and rinsed with water before use clean. 5.2 Analyze the sample of the total amount of elements, add appropriate amount of nitric acid immediately after collection to make the volume fraction of nitric acid reach 1%. Measure 10.00mL after acidification In a 100mL beaker, add 5.0mL nitric acid solution (4.3) and cover with a watch glass. Place it on the hot plate and put it in a near boiling state The sample evaporates to nearly dryness. After cooling, repeat the above operation once, adding nitric acid or perchloric acid if necessary, until the dissolution is complete. After steaming until nearly dry, Remove to cool. Add water to dissolve the residue. If there is any insoluble precipitate, filter through quantitative filter paper, transfer to a 100mL volumetric flask, and add nitric acid solution (4.4) Constant volume, shake well, to be tested. 5.3 When analyzing a sample with dissolved element content, the sample is immediately filtered through a 0.45μm filter membrane after collection, and the obtained filtrate is immediately added to the appropriate amount Nitric acid, so that the nitric acid content reaches 1%. Measure 10.00mL of acidified sample into a 100mL volumetric flask, and dilute to volume with nitric acid solution (4.4) To 100mL, shake well, to be tested. 6 Determination of copper, lead, bismuth, antimony, cobalt, and nickel content---inductively coupled plasma atomic emission spectrometry 6.1 Principle The filtered or digested sample is injected into the inductively coupled plasma emission spectrometer, and the carrier gas is carried into the plasma, and the excited atoms And ion emits atomic spectrum and ion spectrum, and its content is measured by the intensity of element characteristic spectrum. 6.2 Instruments 6.2.1 Inductively coupled plasma atomic emission spectrometer. 6.2.2 The electric heating plate can be adjusted. 6.3 Test procedure 6.3.1 Drawing of working curve Take six 100mL volumetric flasks, add copper, lead, bismuth, antimony, cobalt, nickel mixed standard solution (4.11) 0mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, dilute to 100mL with nitric acid solution (4.4), shake well. According to the optimal working conditions of the instrument, Use a high-purity argon plasma torch at the recommended wavelengths of 324.75nm (copper), 220.35nm (lead), 223.06nm (bismuth), 206.83nm (Antimony), 228.62nm (cobalt), 231.60nm (nickel) of the analytical line signal intensity of the solution. Based on the mass concentration of the element to be measured in the above solution Degree (mg/L) is the abscissa, the signal intensity of the analysis line of the element to be measured is the ordinate, and the working curve is drawn. 6.3.2 Determination On the inductively coupled plasma atomic emission spectrometer, the sample solution was measured under the same conditions as the standard solution series (5.2, 5.3) and the blank solution (take the same volume of water as the sample to prepare the blank solution according to the provisions of 5.2 and 5.3) analysis line signal intensity, from Find the corresponding mass concentration on the working curve. During the sample determination process, if the mass concentration of the element to be tested in the sample exceeds the working curve range, the sample Need to re-measure after dilution. 6.4 Test data processing The total amount of the element to be measured or the dissolved mass concentration ρ, the value is expressed in milligrams per liter (mg/L), calculated according to formula (1). Take the arithmetic average of two parallel determination results as the determination result. The absolute difference between two independent test results obtained under repeatability conditions should not be greater than 10% of the arithmetic mean. 6.5 Detection limit The detection limits of various elements are shown in Table 1. 7.1 Principle The filtered or digested sample is introduced into the air-acetylene flame of the atomic absorption spectrometer, and the absorbance of each element to be measured is measured, and Compare and quantify the absorbance with the corresponding element working curve. 7.2 Equipment 7.2.1 Atomic absorption spectrometer. equipped with flame atomizer, with copper, lead, nickel hollow cathode lamp. 7.2.2 The electric heating plate can be adjusted. 7.3 Test procedure 7.3.1 Drawing of working curve Take six 100mL volumetric flasks, add copper, lead, nickel mixed standard solution (4.12) 0mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, dilute to 100mL with nitric acid solution (4.4), shake well. On the atomic absorption spectrometer, press the optimal working bar of the instrument Set to zero with a blank solution without standard solution, and in the order of mass concentration from low to high, the recommended wavelength is 324.8nm, Measure the absorbance of copper, lead and nickel at 217.0nm and 232.0nm. Take the mass concentration (mg/L) of copper, lead, and nickel in the above solution as horizontal The coordinate, the corresponding absorbance value is the ordinate, and the working curve is drawn. 7.3.2 Determination On the atomic absorption spectrometer, the sample solution (5.2, 5.3) and the blank solution were measured under the same conditions as the standard solution series. The absorbance of the liquid (take the same volume of water as the sample to prepare a blank solution according to the provisions of 5.2 and 5.3), and find the corresponding mass concentration from the working curve degree. In the process of sample determination, if the mass concentration of the element to be tested in the sample exceeds the range of the working curve, the sample needs to be diluted and re-measured. 7.4 Test data processing The total amount of the measured element or the dissolved mass concentration ρ2, the value is expressed in milligrams per liter (mg/L), calculated according to formula (2). Take the arithmetic average of two parallel determination results as the determination result. The absolute difference between two independent test results obtained under repeatability conditions should not be greater than 10% of the arithmetic mean. 7.5 Detection limit The detection limits of various elements are shown in Table 2.

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