HG/T 2415-1993 Determination of trace metals in photographic chemicals - Flame atomic absorption spectrometry
Some standard content:
Chemical Industry Standard of the People's Republic of China
HG / T 2415 -
Photographic chemicals
Determination of trace metals in color-forming agents
Flame atomic absorption spectrometry
Published on March 22, 1993
Ministry of Chemical Industry of the People's Republic of China
Implemented on October 1, 1993
Chemical Industry Standard of the People's Republic of China
Photographic chemicals
Determination of trace metals in color-forming agents
↓Subject content and scope of application
Flame atomic absorption spectrometry
HG /T 2415—93
This standard specifies the method for determining trace metals such as copper, iron, zinc, nickel, lead, chromium, etc. in color formers by flame (acetylene fast air) atomic absorption spectrometry.
This standard is applicable to the determination of trace metals such as copper, iron, zinc, nickel, lead, chromium, etc. in color formers whose ignition residues are soluble in hydrochloric acid or nitric acid. The detection limits are 0.03, 0.20, 0.02, 0.20, 0.10, 0.02μg/mL, respectively. 2 Reference standards:
GB602 Preparation of standard solutions for determination of impurities in chemical reagents GB603 Preparation of preparations and products used in test methods for chemical reagents GB/T4470 Terminology for flame emission, atomic absorption and atomic fluorescence spectrometry GB6682 Specifications and test methods for water used in analytical laboratories GB6819 Dissolved acetylene
GB/T9723 General principles for flame atomic absorption spectrometry of chemical reagents 3 Method summary
The sample is decomposed at high temperature and completely incinerated. Trace metals are dissolved in hydrochloric acid or nitric acid. In an acidic medium, the sample is vaporized by acetylene-air flame on an atomic absorption spectrometer, and the absorbance is determined. The content is calculated using the standard curve method. 4 Reagents and materials
The impurity standard solutions, preparations and products used in this standard are in accordance with GB602, GB 603. The water used in this standard shall meet the specifications of grade II water or grade III water in GB6682. The purity of the reagents used in this standard shall be above analytical grade. The acetylene used in this standard shall meet the requirements of GB6819. 4.1 Compressed air: provided by air compressor. 4.2 Preparation of stock standard solution:
The stock standard solution can be stored for 1 year.
4.2.1 Copper stock standard solution (1 g/L): weigh 1 g of copper standard sample, accurate to 0.1 mg. Dissolve in 5 mL of nitric acid, evaporate to dryness on a water bath, add 5 mL of hydrochloric acid, and evaporate to dryness again. Then dissolve with hydrochloric acid solution (1+99) and dilute to 1000 mL. 4.2.2 Iron stock standard solution (1 g/L): weigh 1 g of iron standard sample, accurate to 0.1 mg. Dissolve in 30 mL of hydrochloric acid solution (I+1), add 20 mL of nitric acid solution (1+1), and dilute to 1000 mL with water. 4.2.3 Zinc stock standard solution (1 g/L): weigh 1 g of zinc standard sample, accurate to 0.1 mg. mL hydrochloric acid solution (1+1), dilute to 1000mL with hydrochloric acid solution (1+99). Approved by the Ministry of Chemical Industry of the People's Republic of China on March 22, 1993 1
Implementation on October 1, 1993
HG/T2415-93
4.2.4 Nickel stock standard solution (1g/L): Prepare in the same way as in 4.2.1. 4.2.5 Lead stock standard solution (1g/L): Weigh 1g of lead standard sample, accurate to 0.1mg. Dissolve in 5mL nitric acid, dilute to 1000mL with nitric acid bath solution (1+99) |tt||4.2.6 Chromium stock standard solution (1g/L): Same as the preparation method in 4.2.3.4.3 Preparation of standard solution:
The following prepared standard solution can be stored for 1 month.4.3.1 Copper, lead and chromium synthetic standard solution (50mg/L): Take 10.00mL of copper, lead and chromium stock standard solution respectively, cover it in a 200mL volumetric bottle, add 2mL of hydrochloric acid solution (1+1), dilute to the scale with water, and mix well.4.3.2 Iron standard solution (50mg/L): Take 10.00mL of iron stock standard solution and put it in a 200mL volumetric bottle. Prepare the following according to the operating steps in 4.3.1.
4.3.3 Zinc standard solution (50mg/L): Same as the preparation method in 4.3.2.4.3.4 Nickel standard solution (50mg/L): Same as the preparation method in 4.3.2. 5. Instruments and devices
5.1 General laboratory instruments.
5.2 Analytical balance: sensitivity is 0.14 g. 5.3 Porcelain snail: capacity is 50 mL, no pollution to samples. 5:4. High temperature furnace: can automatically control the temperature range of 0 ~ 1200 it, air compressor: adjustable pressure range is 0 ~ 10kg/cm*5.5
Flame atomic absorption spectrometer: in accordance with GB9723 regulations5.6
Copper, iron. Hollow cathode lamps for zinc, nickel, lead and chromium: ensure to provide a linear spectrum light source with high brightness and good stability, 57
Atomic absorption working conditions
The working conditions for the determination of copper, iron, zinc, nickel, lead and chromium in colorants are shown in the table below: Measured metal element
Working conditions
Bead length, nm
Slit width, nm
Air flow, L/min
Acetylene flow, L/min
Light source (hollow cathode lamp)
Lamp current, mA
Integration time,
Measuring height, mm
Flame type
Oxidation type
Reduction type
When measuring, the above parameters should be appropriately adjusted according to different instruments to achieve the best measurement conditions for the measured metal element. 2
Drawing of standard curve
HG /T 2415 —93
Pipette 0.20, 0.50, 1.00, 1.50, 2.00mL of the standard solution of the metal element to be measured into each 50mL volumetric flask, add 0.5mL of hydrochloric acid solution (1+1), dilute to the scale with water, and mix well. At the same time, prepare the solvent blank solution, and debug the atomic absorption spectrometer to the best working state according to the atomic absorption working conditions specified in 6. After that, use the solvent blank filter to adjust to zero, repeatedly measure the absorbance of the solution of any concentration mentioned above until it is stable, and measure the absorbance of the above solutions in turn. After each measurement, water should be added to the burner to clean it to avoid interfering with the next measurement. Draw the standard curve with the above solution concentration as the horizontal axis and the corresponding absorbance as the vertical axis. wwW.bzxz.Net
8 Determination steps
Weigh 2 portions of 1g sample, accurate to 0.01, and put them into 50mL porcelain crucibles respectively. Heat on an electric furnace, first adjust the voltage to 220V, and when the sample becomes molten, immediately reduce the voltage to 50V, and then gradually increase the voltage to 220V for heating (strictly prevent a lot of smoke due to over-pressure), until it is completely carbonized (about 6-8h), then put the tower into a high-temperature furnace, slowly increase the temperature, and ash at 500C until it is complete (about 4-8h), then cool to room temperature, absorb 1.00mL of hydrochloric acid or nitric acid and put it into the above garbage containing the burning residue to completely dissolve the residue (warm if necessary). Dilute to 25mL with water, and prepare a blank test solution at the same time. According to the working conditions specified in 6, adjust the atomic absorption spectrometer to the same state as in 7, then measure the blank test solution's absorbance, and then measure the absorbance of the metal element to be measured in the above sample solution three times in parallel (if necessary, it is necessary to measure the absorbance of any concentration used to draw the standard curve to verify the stability of the instrument). Finally, according to the absorbance after blank self-calibration, the concentration of the measured golden phoenix element is checked from the standard curve, and the percentage of the measured metal in the color former is calculated. If the absorbance of the sample solution is too high and exceeds the standard curve, it can be diluted to an appropriate degree with hydrochloric acid solution (1+24) and then measured.
9 Calculation of results
The content of the measured metal impurity (X) in the color former is calculated as follows:CVF×10-6
Wherein:X—the percentage of the measured metal impurity in the color former,%;Concentration of sample solution, μ/mL:
VThe volume of sample solution before dilution, mL;
m—sample mass, g:
FDilution factor, the ratio of the volume of sample solution after dilution to the volume of sample solution before dilution10Allowable difference
The difference in results within the laboratory should not be greater than the allowable difference listed in the following tableContent of metal proton,%
<0. 000 1
0. 000 ~ ~0. 001
>0. 001~0. 002
Allowable difference,%
0. 000 03
0. 000 25
0.000 40
Test report
The test report should include the following contents: HG / T 2415 -
All information about the sample: batch number, date, time and place, model of the instrument used in the test: a.
b. Analysis results and expression method;
c. Abnormal phenomena observed during the measurement; a.
Any operation or optional test condition not included in this standard. 12 Safety matters
An exhaust device should be installed above the burner of the instrument. 12.1
12.2 The two gas sources should be at an appropriate distance from the instrument. Check the pipeline frequently to prevent gas leakage and strictly abide by the relevant operating regulations. Additional Notes: This standard was proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Photosensitive Material Technology Development Center of the Ministry of Chemical Industry. This standard was drafted by the Photosensitive Material Technology Development Center of the Ministry of Electrochemical Industry. Xiamen Photosensitive Material Co., Ltd. and Shanghai Photosensitive Film General Administration participated in the drafting. The main drafters of this standard are Zhang Ping, Yi Keqin, Huang Guiqin, and Ding Peiling. The People's Republic of China Chemical Industry Standard Photographic Chemicals Determination of trace metals in colorants Flame atomic absorption spectrometry HG/T2415-93 Edited by Chemical Industry Standard Editorial Department (Standardization Research Institute of the Ministry of Chemical Industry) Postal Code: [00013 Printing Standardization Research Institute of the Ministry of Chemical Industry Copyright Exclusive Reproduction is prohibited Format 880×12301/[6 Printing Sheet % Number of Words 8000 1993 June First edition in June 1993 First printing in June 1993 Number of copies [—300] Cost of production: RMB 2.20
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