GB/T 4103.2-2000 Chemical analysis methods for lead and lead alloys - Determination of antimony content
Some standard content:
GB/T4103.2:2000
This standard adopts two chemical analysis methods to determine the antimony content in lead and lead alloys. Method 1 is a revision of GB3/T4103.3:1983 "Chemical analysis method for lead-based alloys - Determination of antimony content by crystal violet photometry" and GB/T472.5--1984 "Chemical analysis method for lead ingots - Determination of antimony content by malachite spectrophotometry". Method 2 is a revision of GB3/T4103.4--1983 "Chemical analysis method for lead-based alloys - Determination of antimony content by bromate volumetric method".
This standard complies with:
GB/T1.1--1993
Guidelines for standardization work Unit 1: Rules for drafting and expressing standards Part 1: Basic provisions for standard writing
GB/T1.4-1988 Guidelines for standardization work
Provisions for writing standards for chemical analysis methods
GB/T1467--1978 General principles and general provisions for chemical analysis method standards for metallurgical products GB/T7729---1987 General rules for spectrophotometric methods for chemical analysis of metallurgical products GB/T17433-1998 Basic terminology for chemical analysis of metallurgical products This standard replaces GB/T4103.3-1983, GB/T4103.4--1983 and GB/T472.5--1984 from the date of its entry into force. This standard is proposed by the State Bureau of Nonferrous Metals Industry. This standard is under the jurisdiction of China Nonferrous Metals Industry Standard Metrology and Quality Research Institute. This standard was drafted by Shenyang Smelter and Qubei Copper Processing Plant of Ziyin Nonferrous Metals Company. This standard was drafted by Northwest Copper Processing Company of Baiyin Nonferrous Metals Company. The main drafters of Method 1 of this standard are Zhao Yi; the main drafters of Method 2 are Yu Jianzhong and Yang Ping. 105
1 Scope
National Standard of the People's Republic of China
Chemical analysis methods of lead and lead alloys
Determination of antimony content
Methods for chemical analysis of lead and lead alloys--Determination of antimony contentMethod 1 Determination of antimony content by crystal violet spectrophotometryThis standard specifies the method for the determination of antimony content in lead and lead alloys. GB/T 4103. 2
：1983
代格GB/11103.3
GR/T 1103. 1
G/T 172.5
This standard applies to the determination of antimony content in lead and lead alloys. Determination range: 0.00030%~0.060%, 2 Method Summary
The sample is dissolved with nitric acid or sulfuric acid-potassium sulfate, and sulfuric acid or hydrochloric acid is added to make the main amount of lead form lead sulfate or lead chloride precipitation, which is separated and removed. In the hydrochloric acid medium, toluene is used to extract the blue complex formed by antimony chloride anion and crystal violet, and its absorbance is measured at a wavelength of 610nm on a spectrophotometer. If the sample contains thallium, the coprecipitation of antimony and iron to form hydroxide is separated from it, 3 Reagents
3.1 Anhydrous sodium sulfate.
3.2 Potassium sulfate.
3.3 Toluene.
3.4 Hydrochloric acid (ol.19g/mL).
3.5 Sulfuric acid (p1.84g/ml.).
3.6 Hydrochloric acid (1+1).
3.7 Sulfuric acid (1-+-3).
3.8 Sulfuric acid (1+99).
Nitric acid (1→3).
Phosphoric acid (1-+-4).
Sulfur solution (500g/1.).
Sodium nitrite solution (100g/L).
Saturated ammonium chloride solution.
Ammonium chloride solution (10g/L.).
Ammonia water (1+1).
Ferric chloride solution (10g/L): weigh 1.0g ferric chloride (FeCl:·6I10) and dissolve it in 50ml hydrochloric acid (3.6), dilute to 100ml with sucrose (3.6).
3.17 Stannous fluoride solution (100g/L): weigh 10.0g stannous fluoride (SnCl:·2H2O) and dissolve it in 50ml hydrochloric acid (3.6) with slight heat. Approved by the State Administration of Quality and Technical Supervision on 20000828 106
2000-12-01 implementation
GB/T 4103.2-- 2000
After that, dilute to 100ml with hydrochloric acid (3.6). Prepare it before use. 3.18 Crystal violet solution (2g/1.).
3.19 Antimony standard storage solution: Weigh (1000g) pure antimony, place in a 200ml beaker, add 10mL sulfuric acid (3.5), heat until completely dissolved, cool, transfer to a 1000ml volumetric flask, add 180mL sulfuric acid (1+1), cool. Dilute to scale with water and mix with a spoon. This solution contains 100μg in 1mL.
3.20 Standard solution: Transfer 25 .00mL of standard stock solution of tin in a 500mL volumetric flask, dilute to the mark with hydrochloric acid (3.6), and mix well. This solution contains 5ug in 1mL.
4 Instruments
Spectrophotometer.
5 Analysis steps
5.1 Test materials
Weigh the sample according to Table 1, accurate to 0.0001g. Table 1
Antimony content, %
9.000 300.001 0
≥0. 001 0~0. 004 0
2-0. 004 0~ 0. 010
0. 010~0. 030
>0. 030~ 0. 060
Sample amount·
Dissolved nitric acid
(3.9) volume.mL
Carry out two independent measurements and take the average value. 5.2 Blank test
Carry out a blank test along with the sample.
5.3 Determination
5.3.1 Sample dissolution
5.3.1.1 Total volume of pure lead and lead alloy test solution except tin alloy
Pre-fill the volumetric flask||tt ||Sulfuric acid (3.7) amount, ml
Test solution volume
5.3.1.1.1 Place the sample (5.1) in a 200mL beaker. Add nitric acid according to Table 1, heat at low temperature to dissolve, boil to remove nitrogen oxides, and cool. If the sample contains, proceed as follows in Appendix A. 5.3.1.1.2 Rinse Table III and the beaker wall with water, transfer to a volumetric flask pre-filled with sulfuric acid (3.7) according to Table 1, dilute to scale with water, mix well and let stand for 5 min.
5.3.1.1.3 Take the upper clear liquid according to Table 1 and put it in a 200ml beaker, add 8mL sulfuric acid (3.7), heat and evaporate until white smoke appears and cool to nearly 7 (keep moist).
5.3.1.1.4 Add 10mL hydrochloric acid (3.6), heat at low temperature to dissolve the salts, cool, transfer to a 125mL separatory funnel, wash the beaker with 10mL hydrochloric acid (3.6) in several times, and combine the washings into a separatory funnel. 5.3.1.2 Lead, tin and gold
5.3.1.2.1 Place the sample (5.1) in a 200ml beaker, add 1g potassium sulfate and 10mL sulfuric acid (3.5), heat at high temperature until the sample is completely dissolved, move the beaker to a slightly lower temperature and evaporate to dryness, cool slightly, add 10mL hydrochloric acid (3.6) and heat at low temperature to dissolve the salt, and cool. If the sample contains salts, treat according to Appendix A.
5.3.1.2.2 Transfer the solution to a volumetric flask according to Table 1, wash Table III and the beaker with hydrochloric acid (3.6), combine the washings and pass them into the volumetric flask, dilute to the mark with hydrochloric acid (3.6), mix, and let stand for 5 minutes. 5.3.1.2.3 Take the supernatant according to Table 1 and put it into a 125mL separatory funnel. Add hydrochloric acid (3.6) to a volume of 20ml.5.3.2 Extraction
GB/T 4103.2--2000
Add 12 drops of stannous chloride solution, mix, and let stand for 5min. Add 2mL of sodium nitrite solution, mix, and let stand for 2min. Add 0.50ml of thiourea solution, shake for 10s, immediately add 50ml of water (without shaking), 0.50ml of crystal violet solution, and 25.00ml of toluene, shake for 1min, let stand for 5min, and discard the aqueous phase.
5.3.3 Measurement
Add 1g of anhydrous sodium sulfate and shake several times. Transfer part of the solution into a 1cm absorption III, and use the empty solution accompanying the sample as a reference. Measure its absorbance at a wavelength of 610nm on a spectrophotometer. Find the corresponding antimony amount from the working curve. 5.4 Drawing of the working touch line
5.4.1 Transfer 0.0.501.00, 2.00.3.00.4.00.5.00ml. of antimony standard solution and place it in a set of 125ml. separating funnels, and use hydrochloric acid (3.6) Dilute to 20ml, and proceed as in 5.3.2. 5.4.2 Add 1g of anhydrous sodium sulfate, shake several times, and transfer part of the solution into a 1cm absorbent. Using the reagent blank as a reference, measure its absorbance at a wavelength of 610nm on a spectrophotometer. Draw a working curve with the amount of antimony as the abscissa and the absorbance as the ordinate. 6 Expression of analysis results
Calculate the percentage of antimony according to formula (1):
Sb(%) = m V. X 10
The amount of antimony found from the working curve, g:
Vft: mi .
V.·Total volume of test solution.mL·
V, the volume of test solution taken.mL
mo—the mass of the sample, g.
× 100
The result is expressed to three decimal places. If the content is less than 0.010%, it shall be expressed to four decimal places; if it is less than 0.0010%, it shall be expressed to five decimal places.
7 Allowable Difference
The difference between the analysis results of laboratories shall not be greater than the allowable difference listed in Table 2. Table 2
Antimony content
0. 000 30~0. 000 60
0. 000 60 ~ 0. 001 5
0. 001 5~~0. 003 0
≥ 0. 003 0~ 0. 006 0
20. 006 0~ 0. 010
>0. 010~-0. 020
-0. 020 -0. 040
0. 040-~0. 060
Method 2 Determination of antimony content by cerium sulfate titration
8 Scope
This standard specifies the method for the determination of antimony content in lead and lead edible gold. Allowable difference
0. 000 10
This standard is applicable to the determination of antimony content in lead and lead alloys. Determination range: 0.25%~18.00%. 108
Method Summary
GB/T 4103. 2--2000
The sample is dissolved in sulfuric acid-potassium sulfate, and antimony is reduced to Sb31 with sulfuric acid. In the hydrochloric acid medium, it is titrated with cerium sulfate standard titration solution using methylene blue and methyl orange as indicators.
10 Reagents
10.1 Potassium sulfate.
10.2 Hydrazine sulfate.
10.3 Sulfuric acid (pl.84 g/mL).
10.4 Hydrochloric acid (pl.19 g/ml.).
10.5 Antimony standard solution: Weigh 2.0000g pure antimony (antimony content greater than 99.99%), cover in 400ml. Calcined newspaper. Add 50)ml of stream acid (10.3) to heat and dissolve, boil until the solution is clear, cool. Transfer to a 1000mL volumetric flask, dilute to scale with sulfuric acid (7-+13). Mix well. This solution contains 2mg antimony in 1mL. wwW.bzxz.Net
10.6 Methylene blue solution (1g/L)
10.7 Methyl orange solution (1g/L).
10.8 Standard titration solution of cerium sulfate [c(Ce(SO4)2·4H2O]=0.025mol/L] 10.8.1 Preparation
Weigh 10.0g of sulfuric acid Lc(Ce(SO4)2·4H2O] and place it in a 400ml beaker. Add 200ml of sulfuric acid (8+92) to dissolve it. Transfer it into a 1000ml volumetric flask, dilute it to the mark with sulfuric acid (8+92) and mix well. 10.8.2 Calibration
Weigh 1.000g of pure lead (antimony content not more than 0.005%) and place it in a 500ml conical flask. Add 10.00ml of antimony standard solution (10.5). The following is carried out according to 11.3.2 to 11.3.3. Calculate the actual concentration of the standard titration solution of antimony sulfate according to formula (2): 0.0200
c = (V, - V)× 0. 060 85
Wherein: - actual concentration of antimony sulfate standard titration solution, mol/L; V—volume of antimony sulfate standard titration solution consumed by the test solution during calibration, mL; V,---volume of sulfuric acid standard titration solution consumed by the blank test solution during calibration, mL; (2)
0.06085---mass of the equivalent of 1.00mL sulfuric acid standard titration solution [c(Ce(SO,),4H,O]=1.000mol/1] g/mol
Take three portions for calibration. The range of the volume of sulfuric acid standard titration solution consumed in the calibration should not exceed 0.10mL. Take the average value, otherwise recalibrate.
11 Analysis steps
11.1 Test sample
Weigh the test sample according to Table 3, accurate to 0.0001g. Table 3
0. 25~3. 00
7>3.00--5. 00
>5.00-7. 00
7.00~13.00
>13. 00~17.50
Sample amount g
Carry out 2 independent determinations and take the average value. 11.2 Blank test
GB/T4103.2--2000
Weigh 1.000g of pure lead (antimony content not more than 0.005%) and do a blank test with the sample. 11.3 Determination
11.3.1 Place the sample (11.1) in a 500mL conical flask. 11.3.2 Add 2g potassium sulfate and sulfuric acid according to Table 3, dissolve at high temperature until the sample is completely dissolved, and continue Boil for 20 minutes, cool slightly, add 0.3g sulfuric acid, reduce for 40 minutes at a slight boiling state, and cool. 11.3.3 Use a small amount of water to wash the cup wall, add 50mL of water, immediately add 20mL of hydrochloric acid, 2 drops of methylene salt solution, and 1 drop of methyl orange solution. Under constant shaking, titrate with sulfuric acid standard titration solution until the red color becomes lighter, add 1 drop of methyl orange solution, and slowly titrate until the red color disappears and blue appears as the end point.
12 Expression of analysis results
Calculate the percentage of antimony according to formula (3):
Sb<%) =V)s×0. 60 85 × 100
Formula: Actual concentration of cerium sulfate standard titration solution, mol/L; V—-volume of sulfuric acid standard titration solution consumed by the titration test solution during determination.mL, V. The volume of the cerium sulfate standard titration solution consumed in the titration of the blank test solution during the determination, mL; ... (3)
-The mass of antimony equivalent to 1.00mL of sulfuric acid standard titration solution [c(Ce(SO.),·4Hz0]=1.000mol/L], 0. 060 85-
g/mol;
The mass of the sample, g.
The result should be expressed to two decimal places.
13 Allowable difference
The difference in the analysis results between laboratories should not be greater than the allowable difference listed in Table 4. Table 4
Antimony content
0.25~1.00
>1. 00~3. 00
>3. 00~7. 00
7.00~13. 00
=13, 00~18. 00
Filling tolerance
GB/T4103.2--2000
Appendix A
(Standard Appendix)
Treatment of thallium-containing samples
A1 Transfer the solutions in 5.3.1.1 and 5.3.1.2 into a volumetric flask that has been pre-added with hydrochloric acid (3.4) according to Table 11 (the amount of hydrochloric acid added is 1/10 of the volume of the volumetric flask). Dilute to the mark with water, mix well, and let stand for 5 minutes. A2 Take 1 layer of clear liquid according to Table 1 and put it in a 200mL beaker, add 8mL sulfuric acid (3.7), heat and evaporate until white smoke appears and cool to near dryness (keep moist).
A3 Add 5.0mL ferric chloride solution, 150mL water, 5mL saturated ammonium nitride solution, heat to boil, adjust the solution to pH 5.5~6.5 with ammonia water. Heat to a slight boil for 1 minute , remove and place for 10 minutes. A4 Filter with medium-speed quantitative filter paper, wash the beaker twice with hot ammonium chloride solution, precipitate 4 times, wash the beaker twice with hot water, and precipitate 4 times.
A5 Use 10ml. hot sulfuric acid (3.7) to dissolve the precipitate in the original beaker, wash the filter paper 4 times with hot sulfuric acid (3.8), evaporate the solution to nearly dryness, and cool.
A6 Add 10mL hydrochloric acid (3.6), heat at low temperature to dissolve the salts, cool, transfer to a 125ml separatory funnel, wash the beaker with 10ml. hydrochloric acid (3.6) in batches, and combine the washings in the separatory funnel. A7 Add 12 drops of stannous chloride solution, mix well, and place for 5 minutes. Add 2mL sodium nitrite solution, place for 2 minutes, add 0.50mL thiourea solution, shake for 10s, add 2ml. phosphoric acid, shake 4 to 6 times, immediately add 50ml. water (do not shake), 0.50ml crystal violet solution, 25.00ml toluene, shake for 1min, let stand for 5min, discard the aqueous phase. Follow 5.3.3. 111
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