GB/T 3253.3-2001 Chemical analysis method for antimony - Determination of lead and copper content
Some standard content:
KS 77.123. 60 National Standard of the People's Republic of China GB/T 3253. 7 ~-3253.6 2001 Methods for chemical analysis of antimony 2001- 07 -10 Implementation General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China 2001- 12 -01 Released Model National Standard of the People's Republic of China Method for chemical analysis of antimony Determination of lead and copper cnntents Methods for determination of lead and copper content by atomic absorption spectrometry This standard specifies the method for determination of antimony content CBT 3253.3- 2001
Replace GB/3253.31932
GB, T 3253.4
GB/T 325.5
This standard is applied to the ladder, and the content is determined by shaving. The pool is used for lead 13~U: copper 0330 and 030. 2 Method Summary
After the test seal is decomposed with salt and nitric acid for one year, the rust is removed by repeated addition of aqueous acid. In the dilute hydrochloric acid gel medium, the air acetylene is used to support the peak of the original absorption. The absorbance of lead and molybdenum is measured at 28.1.nm and 321.7nm respectively. Impurities are not measured. 3 Test
3. 1 Hydrochloric acid (ol. 14,/ml.)
3-2 Hydrochloric acid (1+1)
3. 3 Energy (1,42 g/ml.].
3.4 Hydrochloric acid al.48g/inL.
3.5 Lead standard liquid: weigh 1.c05 pure aluminum (99.999%) bone 2Gm1. beaker. Add 3mm1. pin?1+1) Slightly heat to degrade completely, boil the deoxygenated hook, cool and cut. Weigh into 100-capacity bottle with water to dilute to the point, mix. 1 ml of this solution contains 1 mg of lead. 3.6 standard solution: take 1.mL of the standard solution and place it in a 11 mL volumetric flask, add 5% hydrochloric acid (r3), sieve with water to the mark. 1 ml of this solution contains 10% lead. 3.7 standard solution: add 10% pure sodium hydroxide (93.9%) into a 230 mL beaker, add 2 uml of sodium hydroxide (1+1), dissolve in water, transfer to a 10 mL volumetric flask, add 1 um of standard solution containing 13 g of lead. 3.6 standard solution: transfer 1 um of standard solution to a 10 mL volumetric flask, add 5% hydrochloric acid (5.2), sieve with water to the mark, mix, and dissolve in 1 ml. 100 mL of this solution. 4 atomic absorption spectrometer attached, with a hollow lamp. Under the working conditions of the instrument, those that can meet the following requirements can be used. Sensitivity: In the same liquid as the specified concentration, the concentration of the product should not be greater than / less than + c. =3 2g/l..
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China 2001-07·1C approved 20G11201 implementation
CB/T3253.3-2001
Precision: Use a high-volume standard drop solution to test the absorbance of 10 times, and its standard deviation should not exceed 1.0 of the average absorbance. It is necessary to use our natural standard drop solution (. Small sample "standard drop solution") to measure the absorbance 10 times, and its standard deviation should not exceed 1.0 of the average absorbance. The concentration band is divided into five sections, and the ratio of the absorbance difference of the highest section to the absorbance difference of the lowest section should not be less than
. Set the working temperature of the group except recording A (Appendix with reminder) 5 Analysis steps
5.1 Subtraction
Weigh the sample according to Table 1, and the mass efficiency given is c.0001g:
U. (1+-.5. 355
>t.+54~-3.15
**. 15~ .1. 55
J. 35~ . 75
Test-determine the product 1.
Self-measurement and parallel two tests. Take the average of the first test. 5.2 Abandon the test
and do the empty concave test with the sample.
5.3 Determine
the mass efficiency of copper and
o.nn. --..c12
> 2~.. G3G
. a3n~G. 3
2-G. 25~ n. 50
material with fixed volume m
5.3. total (=-1 bone" 3\) ml. burn, add ml. with (3.1), 3L of solution, heat on low temperature furnace to evaporate dry cold add acid: hydrogen waist low humidity heat dry cold add acid cold! . Salt shock \, 1 again heat to Ling, such as human 2. acid (H1) slightly hot solution tiger active, method table 1 regulations to a fixed volume, transfer the network flow 5.3.2 At the wavelengths of 283.nm1.324.7nm of the atomic force microscope, use the word gas-acetylene rapid fire to quickly increase the water to zero: measure the light intensity during the test, and use the measured light absorption card to reduce the light intensity of the test wave to 1. Infer the concentration along the line of the workbook.
5.4 Drawing of the working curve
5.4.1 Preparation of workpiece curve: Take 100ml of C.5.20, 10.00, 15.03.20.00, 25.0%, 3G.90aL of standard lead solution, dilute with water until effective, use air, lack of flame, at the original wavelength of 283.r of the absorbance-spectrophotometer, use water to measure the absorbance of the series of standard reagents to obtain the standard liquid. The absorbance of "zero" micro-waste liquid is measured with the degree of absorption as the mass coordinate and the spread as the numerical coordinate. Preparation work progress: 5.4.2 Preparation of T line drawing: Transfer 0.C.50, 1.00, 1.=C, 2.03.2.50, 3.00L steel standard full liters to a group of 1cm volumetric flasks - add 2ml. Salt and aldehyde are prepared with water, mixed, and the total flame is air-2: the atomic absorption test is not complete? At zero, adjust with water, measure the photometric value of the standard reagent, subtract the absorbance of the standard solution "zero\concentration", and use the energy sensitive rate standard to change the space into the level coordinates and give the industrial curve. 6 Expression of analysis results
According to the formula: 1) Calculate the value of the adjusted mass fraction: tolFb(Cu)
; [Fb(Cu)
, copper content fraction, %:
7 Tolerance
tH/T 3253.3—2001
Make the above-mentioned limit, the separation limit /.: V-full volume of the test drop.mL!
The sample energy mass.
If the analysis result of the laboratory is used, it should not be greater than the tolerance range in Table 2. The post-analysis effect in Table 2
. 010~0. :
2+3 :42~1 51
>3 253~6. 15
2c, 13-~t, 713
2c, *:--c. N0
≥0. 31~.a. 5n
2 G. 51~ 0. 75
3Range
Filling Proof
Method 2
Steel Distribution
n, nos 11--o, ou5 c.
:-f, 55 -0. n20
, n2n--G c3o
0.0n~G.nn
-n, nn-.0. n
>o, 1nfi--n. 2n
. 20~.f. 30
Determination of lead by disulfide spectrophotometry
This standard specifies the determination method for lead in the medium. This standard is applicable to the determination of lead in the medium. Determination range: 001C%~.609 Method summary
Let the material be diluted with hydrochloric acid, nitric acid and sodium hydroxide, in a sodium hydroxide solution, add disulfide solution and separate it by irradiation. Decompose the disulfide solution with the acid, absorb the lead in the filter band with disulfide solution in the medium, and measure its absorbance at a wavelength of 20nm with a spectrophotometer
Take 5g 3.AmR, 2xg copper, 0.5mg alcohol and 3.03m 10 reagent
hot ol.1/mL
salt (111)
can be 1.
10.E potassium hydroxide solution (100+/.),
Note: preparation, pay attention to the use of chemical agents such as manufacturers to avoid the presence of potassium hydroxide in the air, the whole skin protection company original mouse chemical buried or prepared chemical is brought, see the purchase of the cabinet with good ventilation, the organic chemical carrier to remove the red. 1 potassium hydrogen ion 10g m. water add Em hydrogen (Str1 k Yi to 1 000ml. Warm]
GB/I3253.32001
108 Tartar drive liquid (00/) Weigh 400g of tartaric acid aldehyde (KNCH0, HO) in a 10CCm. beaker, add about 5 drops of water, add 2 drops of phenol solution with hydrogen peroxide and mix until red, transfer 1 drop of liquid to 101.1% disulfide solution (10.1% disulfide solution) in batches, extract the organic phase until it is green and white. Remove the organic phase, add 10.2% salt to acidify the solution, add carbon dioxide in batches (about 1U1l each time), wash the disulfide in the aqueous phase until the organic phase is colorless, put the water into a suction filter bottle, and use water to 1 I. Mix well. 09 non-acidic glue liquid 1 weigh 1 benefit model glue in 1C you ring, people range 5m base, witness 1 drop ~ 2 phenol ethanol solution, with hydrogen water to slightly red envelope, transfer to 1CwL separatory funnel, add (about) carbon tetrachloride (about 11 times each time) in batches until the organic matter is green. Discard the organic phase, add salt (1? Avoid the liquid, add (10a) carbon tetrachloride in batches. Select the remaining parent in water until the organic matter is colorless: transfer the aqueous phase to the separation bottle and dilute with water to [GCm filter sentence, 19-10 double forest area will be commercial (0.4 more.) you 2.2 more double flow drying 110mm1 will be in, people's ml. = m After the alkane is completely dissolved, transfer 13 mL of the solution to a separatory tube, add 2 mL of dinitrogen solution, 20 mL of water, let stand for 1 min, and discard the organic phase. Add 1 mL of tetrahydrofuran, add 4 mL of saline, acidify, let stand for stratification, and transfer the organic resin to a separate bottle: add sulfuric acid to protect the surface, and store elsewhere. 10.11% dithiocarbamide (0.04 g/l) carbon dioxide (10.1% dithiocarbamide) solution ... 201mT. hydrochloric acid (10.2) magnetized vibration 1in stand stratification, will be more into brown color pregnant cattle, put Ding anti-noise place. When the mouth preparation. 112 of the cage (1C/L
10.3 broken carefully stored liquid: weigh c.15008 pure aluminum (99.99%) retain 1ccm). In the fire, add 1: +1: heat solution until clear, boil to remove the excited oxide. Collect chicken. Transfer to 1m1. Full bottle, double help rate change, mix with a spoon. This box is slightly,
10.14 lead standard depth: weigh glue 1U.00m second standard storage solution (10.13 + 10 volume or bottle with a scale rate shop leak. This wear multiplied by 1 ml. Contains 11 along
11 receiver
spectrophotometer.
12 Analytical steps
12. 1 Test and
Weigh the test samples according to Table 3 and make sure to weigh 10% of the sample.
The mass of the sample
0.020--0 040
:>0.040--0 :0
The sample was weighed and tested independently for the blank test.
12.3 Determine the amount of
,
>3. 1r~.5. 2
:: 7. 3 -- 2. 5
Recover material tray
u- 201
Test standard.ml.
12.3.1 Place the sample (12.1) in a 1cc cup, add 5mL of alcohol and sodium ion solution. 2ml. Mix. 1m. Dissolve the sample (1.) until it is clear. Obtain about 1mE, remove the oxygen oxides. Remove the sample and cool to room temperature, transfer it to a (T.) container, dilute with water to the mark.
GBT3253.3-2O1
12.3.2 Transfer the sample solution (2.3.1) to a 125L container and add 2cm of water. In the separation process, add 1L hydrochloric acid solution, add 1L sodium tartaric acid to dissolve slightly, add 2 drops of phenol to dissolve, neutralize with 1L hydrogen water until red, add 2 drops of chlorinated acid (12) to make the red color, add 1L of the previous solution, mix and add 1L of sodium tartaric acid to dissolve slightly, add 2 drops of phenol to dissolve, add 1L of sodium tartaric acid ... Separate the layers and collect the organic phase in the second separatory funnel. Sweep the liquid. Add 50 ml of hydrochloric acid (11.3) to the organic phase and set aside to separate the layers. Remove the organic phase. Add 1 g of carbon dioxide and 1 g of nitrogen in the funnel for 1 min. 12.3.5 Collect the organic phase 11 and take the liquid falling into the hollow test tube of the sample as the reference. Measure the light intensity at the spectrophotometer 52:13. Find the corresponding lead content by the working circuit. 12.4 Working circuit 12.4.1 Shift 0.1 .C.2.00,3.(center,4.39.5.00.6.L of the standard solution (10.11)# is placed in a 125L separatory bucket, and the effluent is pressed to about 2cm. Then proceed as in 11.3.3~.12..4. 12.4.2. Transfer part of the organic solution to 1r absorbent medium. Take the blank of the agent as the reference, and measure its absorbance at the center of the spectrophotometer wavelength mr. Take the measurement as the recovery coordinate, and draw the working curve based on the absorbance coordinate. 13. Expression of analysis results
According to the formula: calculated mass fraction,
u(Fb.w,-V.XJO Formula: (Fh: -1% or fraction of the wrong amount. Voucher: m
14 Allowable difference
Sales volume obtained from working curve F, 9;
Total number of formula night M).;
The volume of liquid medicine to be divided into, mL;
R of the sample:
The difference in the analysis results between laboratories should not be greater than the allowable difference listed in Set 4. 4
Needle's mass service efficiency
23. 0) - c. cHc
2-0. 06u ~c- .u
U. . UV.
G- -G- 3
2-0. *-0. 6
Related
15 Scope
BT3253-3—2301
Method 3 Copper reagent spectrophotometric determination of copper content This standard proposes a convenient method for determining the copper content in a sample. This standard is used for the determination of copper content in a sample. Summary of the method: Use acid, nitric acid and sodium ions to prepare a solution. Radiate the solution with copper ions to form a colored compound, which is calcined with dioxygen. The absorbance is measured at a spectrometer at a temperature of 1 m. The solution contains 1(U), 2.5(II), 2.5(II) iron, 10(II) gold and 10(II) silver without interference. 17 Reagents
17.1 Acid (.10 g/ml.),
17.2 Nitrate (.42 μ/ml.),
Hydrogenated water 0.5 g/ml.
Potassium tartrate (8 μg/ml.).
Triethyl dithiocarbamate (copper reagent) solution */T.). 17.7
Z-NDTA solution 50 μg/ml.
Standard sample (10ml),
17.9 Standard sample solution: weigh 0.1 ml of standard sample into a (0ml) cup, add 1 ml of 1% hydroxybenzoic acid (1 ml of solution), boil and remove the oxidative stress, and add 1 ml of 1% hydroxybenzoic acid to the mark, mix, and this sample contains 1 L.
17.1 Standard sample solution: pipette 1 ml of standard sample into a 10 ml cup and dilute to the mark: mix, and this sample contains 1 L.
18 Instruments
Extinction meter
19 Analysis steps
19. 1Dead material
Weigh the test mold according to Table 5 and refine to 3.0UU1%Table
Lang quality score3
24, 00s 10. 012
3.0.2-0, 040
>0.0.40- 11. .0
0. *11-- 0. X1
Jiang carried out two tests as specified, and the average value is shown in Table 19.2 Self-reduction test
can be used as a blank test:
19.3 Determination
GI/r3253.3—2001
19.3.1 Place the sample (19.1> in a 10Fm beaker. Add 3 mL of concentrated potassium hydroxide, 3 mL of antacid, 1 mL of hydrochloric acid. Dissolve in a microfuge until clear, and remove nitrogen compounds. 19.3.7 Transfer the test liquid to a microfuge, use a small Greek sample to withdraw the full scale. 15.3.3 Pipette 2 mL of the test solution according to Table 5, 1 drop of 4-1/4 mol of water, 1 drop of ethanol, neutralize with chlorine water until red, 2 drops of copper reagent. Mix, and then add: 3 drops of m1. dichloromethane flow, stir for 2 min. Let stand and separate. 15.3.5 Take part of the organic matter and put it into 1m absorbance, take the test material with the same material as reference, and measure its absorbance at 44nm of the spectrometer. The corresponding working curve is as follows: 15.4 Working end preparation
19.4.- Transfer 0.1.00.2.6c, 3.004.00.5.03.5.00l. Standard liquid volume: -6aT drop, reduce to 2mL with water, add 1m potassium ion solution, and proceed as in 19.3.4. 19.4.2 Take part of the organic matter and put it into 1m absorbance, take the reagent blank as reference, and measure its absorbance at 44nm of the spectrometer wavelength. Take the sample as the coordinate, and prepare the working curve with the absorbance coordinate. 20
Analysis results
Calculate the copper mass fraction according to formula 3):
m, -V, × 10 -
+, iiCu?
21 Allowable difference
Any fraction of the system:
The amount of copper zeroed out on the working line;
The total weight of the test solution, m.
The rest of the test solution, mL;
The mass of the test solution:
The difference between the analysis stations in the laboratory should not be too large. The allowable difference table listed in Table 6 below
Steel's final fraction
0. 00: 0--C 005 Cwww.bzxz.net
≥ 0, 005 0. 0. 025
n, o4o-0. oc5
6. u- ~0. . tu
. 1-. 2t
2 2~ 3
Yuan Xu Award
GD/T3253-3—2001
Appendix A
(Differential Recording)
Instrument Working Conditions
Use WFX-201 Atomic Absorption Spectrometer 1 The working conditions are shown in Table A1. Table A1
.124 7
Light Falling Wine Band
Sensing Evil
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