GB/T 26522-2026Refined nickel chloride (English PDF)

6.3.1 Weight method (arbitration method)

6.3.1.1 Principle In ammoniacal solutions, tartaric acid is added to form soluble complexes with impurities such as iron and aluminum to eliminate interference. This is achieved using dimethylglyoxime and nickel. A red precipitate of nickel dimethylglyoxime was formed. The precipitate was filtered, washed, dried, and weighed to calculate the nickel content.

6.3.1.2 Reagents or materials 6.3.1.2.1 Ethanol solution. 1 4. 6.3.1.2.2 Hydrochloric acid solution. 1 1. 6.3.1.2.3 Ammonia solution. 1 1. 6.3.1.2.4 Ammonium chloride solution..200 g/L. 6.3.1.2.5 Tartaric acid solution..200g/L. 6.3.1.2.6 Dimethylglyoxime ethanol solution. 10 g/L.

6.3.1.3 Instruments and Equipment 6.3.1.3.1 Glass sand crucible. 5µm~15µm. 6.3.1.3.2 Electric constant temperature drying oven. The temperature can be controlled at 105°C±2°C.

6.3.1.4 Test Procedure Weigh approximately

2.0 g of sample, accurate to 0.0002 g, and place it in a 250 mL beaker. Add 2 mL of hydrochloric acid solution and 50 mL of water, and heat to [temperature missing]. Dissolve, cool to room temperature, transfer completely to a 100 mL volumetric flask, dilute with water to the mark, and shake well. Transfer 10 mL of the test solution to a 400 mL beaker using a pipette, add 150 mL of water, 5 mL of ammonium chloride solution, and 5 mL of alcohol. Prepare a petrolic acid solution, cover with a watch glass, and heat to boiling. Cool to 70°C-80°C, then slowly add 30 mL of dimethyl ethylene glycol while continuously stirring. Prepare an aldehyde oxime ethanol solution by adding ammonia solution dropwise to adjust the pH to 8-9 (test with precise pH paper), then add an excess of 1-2 mL. Hold at 70°C~80°C for 30 min, filter through a glass sand crucible that has been dried to constant mass at 105°C±2°C, and wash with ethanol solution. Dry at 105°C±2°C for 4 to 5 times until the quality is constant.

6.3.1.5 Experimental Data Processing The nickel content is expressed as the mass fraction of nickel (Ni), w1, and is calculated according to formula (1).

6.3.2 Complexometric Titration

6.3.2.1 Principle The sample was decomposed with acid, and impurities such as copper, iron, calcium, and magnesium were masked with potassium sodium tartrate, ammonium fluoride, and sodium thiosulfate at an ammoniacal pH of 8-9. In the solution, ammonium purpurate was used as an indicator, and the solution was titrated with standard disodium ethylenediaminetetraacetate solution until the solution turned purple-red.

6.3.2.2 Reagents or materials 6.3.2.2.1 Ammonium fluoride. 6.3.2.2.2 Hydrochloric acid solution. 1 1. 6.3.2.2.3 Ammonia solution. 1 1. 6.3.2.2.4 Potassium sodium tartrate solution. 150 g/L. 6.3.2.2.5 Sodium thiosulfate solution. 500 g/L. 6.3.2.2.6 Standard titration solution of disodium ethylenediaminetetraacetate. c(EDTA)~0.02mol/L. 6.3.2.2.7 Ammonium purpurate indicator. 1g ammonium purpurate and 100g sodium chloride (dried at 105°C±2°C for 2h and cooled in a desiccator) However, they were mixed and ground finely in a mortar.

6.3.2.3 Test Procedure 6.3.2.3.1 Preparation of test solution Weigh approximately

1.0 g of sample, accurate to 0.0002 g, and place it in a 250 mL beaker. Add 50 mL of water and 2 mL of hydrochloric acid solution, and heat to dissolve. Solution. After cooling to room temperature, completely transfer the solution to a 250mL volumetric flask, dilute with water to the mark, and shake well. 6.3.2.3.2 Test Transfer 25 mL of the test solution to a 500 mL Erlenmeyer flask, add 1 g to 2 g of ammonium fluoride and 10 mL of potassium sodium tartrate solution. Add 15 mL of sodium thiosulfate solution and

0.1 g of ammonium purpurate indicator, shake well, and then add ammonia solution dropwise until the solution turns yellow. Then, use ethylenediaminetetraacetic acid (EDTA) dimethyl ether... Titrate with sodium standard solution until the solution turns orange-yellow, then add ammonia solution until the solution turns yellow, and continue titrating with disodium ethylenediaminetetraacetate standard solution. Titrate with the standard titrant solution. After the solution color deepens, add ammonia solution until the solution turns yellow, then titrate with disodium ethylenediaminetetraacetate standard. Titrate the solution repeatedly until the solution turns purple-red, which is the endpoint.

6.3.2.4 Experimental Data Processing The nickel content is expressed as the mass fraction of nickel (Ni), w1, and is calculated according to formula (2).

6.4 Determination of Cobalt (Co), Zinc (Zn), Iron (Fe), Copper (Cu), Lead (Pb), Cadmium (Cd), Chromium (Cr), Manganese (Mn), Calcium (Ca), and Magnesium (Mg)

6.4.1 Principle In nitric acid medium, the content of the analyte was determined by inductively coupled plasma atomic emission spectrometry using the standard curve method.

6.4.2 Reagents or materials

6.4.2.1 Nitric acid solution. 1.1, prepared using superior grade nitric acid.

6.4.2.2 Nickel-based solution. rho(Ni) = 20 g/L, weigh approximately (20.0 ± 0.1) g of metallic nickel (nickel mass fraction not less than 99.99%); cobalt The mass fractions of Co, zinc (Zn), iron (Fe), copper (Cu), lead (Pb), cadmium (Cd), chromium (Cr), manganese (Mn), calcium (Ca), and magnesium (Mg) are all not greater than [amount missing]. 0.0002% was placed in a 400mL beaker; a small amount of water was added to moisten the solution, and 150mL of nitric acid solution was slowly added. The mixture was heated until completely dissolved; it was then cooled to room temperature. Then, transfer it to a 1000mL volumetric flask, dilute with water to the mark, and shake well.

6.4.2.3 Standard stock solutions for cobalt, zinc, iron, copper, lead, cadmium, chromium, manganese, calcium, and magnesium. 1 mL of solution contains cobalt (Co), zinc (Zn), iron (Fe), and copper. 1 mg each of Cu, Pb, Cd, Cr, Mn, Ca, and Mg. Prepare each element according to HG/T 3696.2. Standard stock solutions, or elemental standard stock solutions prepared using certified reference materials.

6.4.2.4 Mixed standard solution A. 1 mL of solution contains cobalt (Co), zinc (Zn), iron (Fe), copper (Cu), lead (Pb), cadmium (Cd), chromium (Cr), and manganese. (Mn) were

0.01 mg each. Using a pipette,

1.0 mL of solutions prepared according to HG/T 3696.2 were respectively used for cobalt, zinc, iron, copper, lead, cadmium, chromium, and manganese. Prepare the standard stock solution in a 100 mL volumetric flask; dilute to the mark with water and mix well. Prepare the solution fresh before use.

6.4.2.5 Mixed standard solution B. 1 mL of solution contains

0.05 mg of calcium (Ca) and

0.05 mg of magnesium (Mg). Use a pipette to transfer

5.0 mL of each solution... Prepare standard stock solutions of calcium and magnesium according to HG/T 3696.2, and place them in a 100 mL volumetric flask; dilute with water to the mark and shake well. Prepare the solution immediately before use.

6.4.2.6 Water. Class II water as specified in GB/T 6682-2008.

6.4.3 Instruments and Equipment Inductively coupled plasma atomic emission spectrometer. should meet the requirements of JJG768.

6.4.4.1 Plotting the Standard Curve Transfer

0.00 mL,

0.50 mL,

8.00 mL of mixed standard solution A and mixed standard solution A, respectively. Liquid B was placed in six 100 mL volumetric flasks; then 10 mL of nickel matrix solution and 2 mL of nitric acid solution were added to each flask, and the solutions were diluted with water to the mark. Shake well. Set the inductively coupled plasma atomic emission spectrometer to its optimal operating conditions and measure the analytes at the recommended wavelengths listed in Table 2. The spectral intensities of its standard solutions. Plotting the mass concentration (mg/L) of the analyte in each standard solution on the x-axis, the corresponding spectral intensities are... Use the ordinate to plot the standard curves for each element to be measured.

6.4.4.2 Test Weigh

1.0 g of sample, accurate to 0.0001 g, and place it in a 100 mL beaker; add an appropriate amount of water, boil to dissolve; after cooling, add... Transfer 2 mL of nitric acid solution to a 100 mL volumetric flask, add water to the mark, and shake well. Simultaneously perform a blank test. The blank test solution contains the same types and amounts of reagents as the test solution, except that no sample is added. The spectral intensities of each analyte in the test solution were measured, and the corresponding values were determined from the standard curve based on the measured spectral intensities. Mass concentration of the element to be measured.

6.4.5 Experimental Data Processing The content of each element to be tested in the test solution is expressed as the mass fraction (wi) of the element to be tested, and is calculated according to formula (3).

6.5 Determination of Sodium Content

6.5.1 Principle In nitric acid medium, the sodium content was determined using the standard curve method and inductively coupled plasma atomic emission spectrometry.

6.5.2 Reagents or materials

6.5.2.1 Nitric acid solution. 1 1, prepared using superior grade nitric acid.

6.5.2.2 Sodium Standard Stock Solution. 1 mL of solution contains 1 mg of sodium (Na). Prepare the sodium standard stock solution according to HG/T 3696.2, or use a suitable solution. Prepare elemental standard stock solutions using standard reference materials.

6.5.2.3 Sodium standard solution. 1 mL of the solution contains

0.1 mg of sodium (Na). Use a pipette to transfer 10 mL of the sodium standard stock solution into a 100 mL container. Dilute to the mark with water in a volumetric flask and shake well. Prepare the solution fresh before use.

6.5.2.4 Water that meets the requirements of GB/T 6682-2008 as Grade II.

6.5.3 Instruments and Equipment Inductively coupled plasma atomic emission spectrometer.

6.5.4.1 Plotting the Standard Curve Use a pipette to transfer

0.00 mL,

0.50 mL,

8.00 mL of sodium standard solution, respectively, into six containers. In a 100mL volumetric flask, add 10mL of nickel-based solution and 2mL of nitric acid solution, dilute to the mark with water, and mix well. Then, connect the inductively coupled plasma... The daughter emission spectrometer was adjusted to optimal operating conditions, zeroed using a standard blank solution, and the spectrum of the standard solution was measured at a wavelength of 589.592 nm. Intensity. A standard curve was plotted with sodium mass concentration (mg/L) on the x-axis and the corresponding spectral intensity on the y-axis.

6.5.4.2 Test Weigh approximately

1.0 g of the sample, accurate to 0.0002 g, and place it in a 100 mL beaker. Add an appropriate amount of water and stir until completely dissolved. Add... Transfer 2 mL of nitric acid solution to a 100 mL volumetric flask, add water to the mark, and shake well. Simultaneously perform a blank test. The blank test solution contains the same types and amounts of reagents as the test solution, except that no sample is added. The spectral intensities of sodium in the test solution and blank test solution were measured, and the phase ratio was determined from the standard curve based on the measured spectral intensities. The corresponding sodium mass concentration.

6.5.5 Experimental Data Processing The sodium content is expressed as the mass fraction of sodium (Na) w2, and is calculated according to formula (4).

6.6.1 Atomic Fluorescence Spectroscopy (Arbitration)

6.6.1.1 Principle In an acidic solution, pentavalent arsenic is pre-reduced to trivalent arsenic using thiourea-ascorbic acid. Then, in a hydride generator, the arsenic is further reduced to trivalent arsenic by potassium borohydride. The fluorescence intensity of the hydride was measured using an atomic fluorescence spectrometer.

6.6.1.2 Reagents or materials 6.6.1.2.1 Hydrochloric acid solution. 1 1. 6.6.1.2.2 Hydrochloric acid solution. 5 95. 6.6.1.2.3 Thiourea-Ascorbic Acid Solution. Weigh 10g thiourea and 10g ascorbic acid, dissolve them in water, and transfer the solution to a 100mL volumetric flask. Dilute with water to the mark, mix well, and prepare the solution fresh each time you use it. 6.6.1.2.4 Potassium borohydride solution. Weigh 2.5g of potassium hydroxide, dissolve it in an appropriate amount of water, then add 10g of potassium borohydride and dissolve completely before transferring. Pour into a 500mL volumetric flask, dilute with water to the mark, mix well, and prepare the solution immediately before use. 6.6.1.2.5 Arsenic Standard Solution A. 1 mL of this solution contains

0.01 mg of arsenic (As). Use a pipette to transfer 1 mL of the solution prepared according to HG/T 3696.2. Prepare a standard stock solution of arsenic impurities, or a standard stock solution prepared using certified reference materials, and place it in a 100 mL volumetric flask, then dilute to the mark. Shake well. 6.6.1.2.6 Arsenic Standard Solution B. 1 mL of this solution contains

0.001 mg of arsenic (As). Use a pipette to transfer 10 mL of arsenic standard solution A into a container... Dilute to the mark in a 100mL volumetric flask and mix well. Prepare the solution fresh before use.

6.6.1.3 Instruments and Equipment Atomic fluorescence spectrometer. equipped with a high-intensity arsenic hollow cathode lamp.

6.6.1.4 Test Procedure 6.6.1.4.1 Plotting the Standard Curve Transfer

0.00 mL,

0.05 mL,

0.10 mL,

0.20 mL,

0.40 mL, and

0.80 mL of arsenic standard solution B into six 100 mL aliquots. Add 10 mL of hydrochloric acid solution (6.6.1.2.1) and 10 mL of thiourea-ascorbic acid solution to the volumetric flasks, respectively. Let stand for 30 minutes, then dilute with water. Dispense to the mark and shake well. An atomic fluorescence spectrometer was used, with a high-intensity arsenic hollow cathode lamp as the light source, potassium borohydride as the reducing agent, and hydrochloric acid solution (6.6.1.2.2) as the carrier. Run the solution through the instrument to its optimal operating conditions and measure the fluorescence value. Subtract the blank test value from the fluorescence value of each arsenic standard working solution. A standard curve was plotted with the fluorescence value of the solution, using the mass concentration of arsenic (mg/L) as the x-axis and the fluorescence value as the y-axis. 6.6.1.4.2 Test Weigh approximately

1.0 g of sample, accurate to 0.0002 g. Place in a 100 mL beaker and dissolve in water. Transfer completely to a 100 mL volumetric flask. Add 10 mL of hydrochloric acid solution (6.6.1.2.1) and 10 mL of thiourea-ascorbic acid solution to the bottle, let stand for 30 minutes, then dilute with water to the mark. Shake well. Atomic fluorescence spectrometry was used with a high-intensity arsenic hollow cathode lamp as the light source, potassium borohydride-sodium hydroxide solution as the reducing agent, and hydrochloric acid solution as the reducing agent. Liquid (6.6.1.2.2) was used as the carrier solution. The instrument was adjusted to its optimal operating conditions, and after stabilization, its fluorescence value was measured. The fluorescence value was then obtained from the standard curve. Find out the corresponding mass concentration of arsenic. Simultaneously perform a blank test. The blank test sol...