GB/T 4375.12-1984 Chemical analysis of gallium - Determination of lead, copper, nickel, aluminum, indium and zinc by chemical spectrometry
Some standard content:
National Standard of the People's Republic of China
Chemical analysis methods
Chemical spectroscopic method for the determination of lead, copper,' nickel,aluminum, indium and zinc contentsUDC 669.871
GB 4375.12--84
This standard is applicable to the simultaneous determination of lead, copper, nickel, aluminum, steel and zinc in gallium (99.999%). Determination range: lead 5×10-5～3×10~1%;
copper 5×10=5～3×10-4%;
nickel 5×10-6~5×10-5%
aluminum 5×10-6~5×10-5%
steel 1×10-5～1×10-4%;
zinc 1×10=5～1×10=4%.
This standard complies with GB1467-78 "General Principles and General Provisions of Chemical Analysis Methods for Metallurgical Products". 1 Method Summary
The sample is dissolved in hydrochloric acid and nitric acid. In 7.5N hydrochloric acid medium, the main gallium is extracted and separated with isocyanate, and the impurities (lead, copper, nickel, aluminum, steel, zinc) enriched in the aqueous phase are excited by spark light source or AC arc light source by solution residue method and spectral determination is carried out. 2 Reagents
2.1 Hydrochloric acid (specific gravity 1.19): calibrate its concentration after distillation and purification at 95℃ in a quartz distiller. 2.2 Hydrochloric acid (7.5N): Prepare with hydrochloric acid (2.1). 2.3 Hydrochloric acid (6N): Prepare with hydrochloric acid (2.1). 2.4 Nitric acid (specific gravity 1.42): Distill and purify with a quartz distiller at 120℃. 2.5 Isopropyl ether: In a separatory funnel, first use 10% hydroxylamine hydrochloride solution or 20% ammonium ferrous sulfate solution to shake and wash to remove peroxide, then transfer to a distillation flask, distill and purify in a water bath at 80℃, and collect the distillate at 67-69℃. Saturate with hydrochloric acid (2.2) before use. 2.6 Deionized water: conductivity greater than 10M2. 2.7 Polystyrene benzene solution (1.5%).
2.8 Lead standard storage solution: Weigh 1.000g pure lead (99.9% or more), place in a 300ml beaker1, add 10ml nitric acid (1+1), dissolve at low temperature, evaporate the solution to a small volume, remove and cool, transfer to a 1000ml volumetric flask4, add 100ml hydrochloric acid (specific gravity 1.19), dilute to scale with water (2.6), and mix. This solution contains 1.0mg lead per ml. 2.9 Copper standard storage solution: Weigh 1.000g pure copper (99.9% 1:), place in a 300ml beaker, add 10ml nitric acid (1+1), dissolve at low temperature, evaporate the solution to a small volume, remove and cool, transfer to a 1000ml volumetric flask, add 100ml hydrochloric acid (specific gravity 1.19), dilute to scale with water (2.6), and mix. This solution contains 1.0mg copper per ml. 2.10 Nickel standard storage solution: Weigh 1.000g pure nickel (99.9% or more) and place it in a 300ml beaker. Add 10ml nitric acid. After low temperature dissolution, evaporate the solution to a small volume, remove and cool, transfer to a 100ml container, add 10ml hydrochloric acid (specific gravity 1.19), dilute to scale with water (2.6), and mix. This solution contains 1.0mg nickel in 1ml. 2.11 Standard stock solution: weigh 1.000g pure sodium (99.9% or above), put it in a 300ml beaker, add 20ml hydrochloric acid (specific gravity 1.19), add 1-2ml nitric acid (specific gravity 1.42), dissolve at low temperature, transfer to a 1000ml container, add 80ml hydrochloric acid (specific gravity 1.19), dilute to scale with water (2.6), mix. This solution contains 1.0mg calcium per ml. 2.12 Standard stock solution: weigh 1.00g sodium (99.9% or above), put it in a 300ml beaker, add 2ml hydrochloric acid (specific gravity 1.19), dissolve at low temperature, remove and cool, transfer to a 1000ml container, add 80ml hydrochloric acid (specific gravity 1.19), dilute to scale with water (2.6), mix. This solution contains 1.\mg per ml. 2.13 Zinc standard stock solution: Weigh 1.000g pure (99.9% 1), place in a 3ml beaker, add 20ml acid (specific gravity 1.19), dissolve at low temperature, remove and cool, transfer to a 100ml volumetric flask, add 80ml hydrochloric acid (specific gravity 1.19), dilute to scale with water (2.6), and mix. This solution contains 1.mg zinc per ml. 2.14 Mixed standard solution of lead, copper, nickel, aluminum, steel, and zinc: Transfer 10.0W)ml of lead, copper, nickel, steel, and zinc standard stock solutions (2.8-2.13) respectively, place in a 100ml volumetric flask, add 10ml acid (2.1), dilute to scale with water (2.6), and mix. This solution contains 100μg each of lead, copper, nickel, aluminum, steel, and zinc per ml. 2.15 Mixed standard solution of lead, copper, nickel, aluminum, steel and zinc: Pipette 5.00 ml of mixed standard solution (2.14), place in a 50 ml container, add 5 ml of hydrochloric acid (2.1), dilute to full scale with water (2.6), and mix. This solution contains 10 μg each of lead, copper, nickel, aluminum, steel and zinc in 1 ml.
2.16 Mixed standard solution of lead, copper, nickel, aluminum, steel and zinc: Pipette 5.00 ml of mixed standard solution (2.15), place in a 50 ml container, add 5 ml of hydrochloric acid (2.1), dilute to full scale with water (2.6), and mix. This solution contains 1 μg each of lead, copper, nickel, aluminum, steel and zinc in 1 ml.
2.17 Bismuth standard stock solution: Weigh 1.000g pure bismuth (99.9% 1:), place in a 300ml beaker, add 10ml nitric acid (1+1), dissolve at low temperature, evaporate the solution to a small volume, remove and cool, transfer to a 1000ml volumetric flask, add 100ml hydrochloric acid (specific gravity 1.19), dilute to scale with water (2.6), mix. This solution contains 1.0mg bismuth per ml. 2.18 Ortho standard stock solution: Weigh 1.9067g sodium chloride (super pure) previously burned at 400-450C until no explosion, dissolve in water, transfer to a 1000ml volumetric flask, add 100ml hydrochloric acid (specific gravity 1.19), dilute to scale with water (2.6), mix. This solution contains 1.0mg bismuth per ml.
2.19 Bismuth and potassium mixed standard solution: Take 10.00ml bismuth standard stock solution (2.17) and 20.0ml potassium standard stock solution (2.18), put them into a 100ml volumetric flask, add 10ml hydrochloric acid (2.1), dilute to scale with water (2.6), and mix. This solution contains 100ug bismuth and 200μg potassium in 1ml. It is used as the internal standard solution for spark light source excitation. 2.20 Sodium chloride standard solution: Weigh 1.7787g high-purity sodium chloride (BaCl2·2H,O), dissolve it in boiled water, cool it and transfer it into a 1000ml volumetric flask, add 100m hydrochloric acid (specific gravity 1.19), dilute to scale with water (2.6), and mix well. This solution contains 1.0mg potassium in 1ml. It is used as the internal standard solution for arc light source excitation. 3 Instruments and Materials
3.1 Medium-sized camera: wavelength range 200~3500A, reciprocal linear dispersion 3.9~2.2Amm. 3.2 AC continuous arc generator or high and low spark generator. 3.3 Microphotometer.
3.4 Electrode: spectrally pure, 6mm thick, 25mm long flat-head electrode. Seal with 1 drop of polystyrene benzene solution (2.7) before use.
3.5 Photosensitive plate: spectral ultraviolet type.
4 Analysis Steps
4.1 Determination Number
Weigh 3 samples for determination and take the average value. 314
4.2 Sample Quantity
Weigh 0.5000g sample.
4.3 Empty Test
Carry out 3 empty tests with the sample.
4.4 Determination
4.4.1 Enrichment of impurity ferric oxide
GB 4375.12-84
Put the sample (4.2) in a 50ml English beaker, add 2.5ml hydrochloric acid (2.1) and 0.5ml nitric acid (2.4), cover with Table III and heat on an electric furnace, gradually raise the temperature to 80 (to make the sample completely dissolved, continue to raise the temperature to 140°C, evaporate the solution to a small volume, add a small amount of hydrochloric acid (2.1) Remove excess nitric acid. Remove, add 5 ml of hydrochloric acid (2.2), cool, transfer to a 50 ml separatory funnel, rinse the beaker with hydrochloric acid (2.2), and add the washing liquid to the separatory funnel for half an hour to make the final volume 10 ml. Add 10 ml of isopropyl ether (2.5), shake for 5 minutes, let stand and separate, transfer the water rod to another separatory funnel, and repeat the extraction with 10 ml of isopropyl ether (2.5). Transfer the water rod to a 10 ml crucible and add the internal standard solution [using a spark light source, add 0.05 ml of the mixed standard solution (2.19); using an arc light source, add 0.02 ml of the standard solution (2.20)]. Place the quartz glass in a dustproof evaporator, ignite under infrared light, add 0.1ml hydrochloric acid (2.3) while hot to dissolve the residue, pipette the residue solution onto the head of the counter electrode (3.4) in a plexiglass dust cover, and bake it for 1 hour under infrared light for spectrum photography. 4.4.2 Preparation of standard series
According to the different light sources used, use a pipette to drop a certain amount of different internal standard solutions (the amount of internal standard solution is the same as that of 4.4.1) onto the head of each pair of electrodes (3.4), and bake it for 1 hour under infrared light. Then drop 0.10, 0.03, 0.01ml of mixed standard solution (2.14), 0.03, 0.01ml of mixed standard solution (2.15), 0.03, 0.01ml of mixed standard solution (2.16), and bake it for 1 hour under infrared light, and then take spectrum with the enriched sample.
4.4.3 Spectral measurement conditions
Spectrograph: lens illumination system, slit 10μm, middle light bar height 5mm. Light source: high voltage spark generator, synchronous QODA controlled discharge, voltage 22010700V, capacitance 6nF, inductance 1.5mH, twilight time 605, AC arc generator, using AC continuous arc, current 5A, exposure time 30s. Photographic plate processing: developer and photoconductive solution are prepared according to the instructions for the photosensitive plate. Develop at 20±1C, fix, rinse in running water, and dry.
Blackness measurement: Use a microphotometer (S scale) to measure the illumination of each analysis line pair. See Table 1 for the analysis line pairs:
Pb2823.19
Cu282.1.37
N; 3,82
A1 31182.16
In3256.19
7,n 33 15,12
Spark light source
Bi 2897.98
Bi 2897.98
Bi 2897.98
: 2897.98
B:2897.98
1: 2897.98
Arc light source
Ba 3071.59
Ba 3071.59
Ba 3071.59
Ba 3171.59
Ba3n71.59
Ba 3071.59
Calculation of analysis results
GB 4375.12—84
From the emulsion characteristic curve drawn, convert the blackness value of the analysis line pair into the logarithm of the intensity ratio (1g for plotting and plotting the curve.
Calculate the percentage of each impurity according to the following formula: X(%)
m2 -mi
mo×106
The most impurity element found on the plotting curve, ug: Formula: m
ml——the amount of impurity elements in the sample obtained from the curve, μg: mo
Allowance difference
Sample amount, g.
The difference between the analysis results of laboratories should not be greater than the allowable difference listed in Table 2. Table 2
Determination elements
5×10 -5~1×10 +
21×10 *+~3×10 *4
5×10 *5~1×10-4
*1×10**~3×10**
5×10 ~9×10\#
*9×10 ~2×10*5
*2×10-5~5×105
5×10-6~9×10~6
9×10*6~2×10-5
*2×10 ~5×10-5
1×10 5~3×10°5
-3×10 5~7×10 5
5~1×10~4
5~3×10
-3×10 5~7×10 5
5~1×10
, to lg
2×10 +
7×10~3
2×10*4
1×105
6×10\6
1×10-
2×105
3×10~5
3×10~5
niKAoNiKAca-
Additional Notes:
GB4375.12--84
This standard was proposed by China Nonferrous Metals Corporation. This standard was drafted by the Nonferrous Metals Research Institute of China Nonferrous Metals Corporation. The main drafters of this standard are Chen Jiaying and Zhong Xiuxia.31712—84
From the emulsion characteristic curve drawn, convert the blackness value of the analysis line pair into the logarithm of the intensity ratio (1g for plotting, and draw the plotting curve.
Calculate the percentage of each impurity according to the following formula: X(%)
m2 -mi
mo×106
The maximum impurity element found on the plotting curve, ug: Formula: m
ml——The amount of impurity elements accompanying the sample found on the plotting curve, μg: mo
Allowance difference
Sample amount, g.
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 2. Table 2
Determination elements
5×10 -5~1×10 +
21×10 *+~3×10 *4
5×10 *5~1×10-4
*1×10**~3×10**
5×10 ~9×10\#
*9×10 ~2×10*5
*2×10-5~5×105
5×10-6~9×10~6
9×10*6~2×10-5
*2×10 ~5×10-5
1×10 5~3×10°5
-3×10 5~7×10 5
5~1×10~4
5~3×10
-3×10 5~7×10 5
5~1×10
, with lg
2×10 +
7×10~3
2×10*4
1×105
6×10\6
1×10-
2×105
3×10~5
3×10~5
niKAoNiKAca-
Additional remarks:
GB4375.12--84
This standard was proposed by China Nonferrous Metals Corporation. This standard was drafted by the Nonferrous Metals Research Institute of China Nonferrous Metals Corporation. The main drafters of this standard are Chen Jiaying and Zhong Xiuxia.31712—84
From the emulsion characteristic curve drawn, convert the blackness value of the analysis line pair into the logarithm of the intensity ratio (1g for plotting, and draw the plotting curve.
Calculate the percentage of each impurity according to the following formula: X(%)
m2 -mi
mo×106
The maximum impurity element found on the plotting curve, ug: Formula: m
ml——The amount of impurity elements accompanying the sample found on the plotting curve, μg: mo
Allowance difference
Sample amount, g.
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 2. Table 2bzxz.net
Determination elements
5×10 -5~1×10 +
21×10 *+~3×10 *4
5×10 *5~1×10-4
*1×10**~3×10**
5×10 ~9×10\#
*9×10 ~2×10*5
*2×10-5~5×105
5×10-6~9×10~6
9×10*6~2×10-5
*2×10 ~5×10-5
1×10 5~3×10°5
-3×10 5~7×10 5
5~1×10~4
5~3×10
-3×10 5~7×10 5
5~1×10
, with lg
2×10 +
7×10~3
2×10*4
1×105
6×10\6
1×10-
2×105
3×10~5
3×10~5
niKAoNiKAca-
Additional remarks:
GB4375.12--84
This standard was proposed by China Nonferrous Metals Corporation. This standard was drafted by the Nonferrous Metals Research Institute of China Nonferrous Metals Corporation. The main drafters of this standard are Chen Jiaying and Zhong Xiuxia.317
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