Some standard content:
National Standard of the People's Republic of China
Polymeric ferric sulfate
Water purification agent
Water riarfying agent-Polymeric ferric strlrate1 Subject content per scope of application
GB 14591 --- 93| |tt||This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation, storage, and safety requirements for polyferric sulfate products.
This standard applies to polymeric ferric sulfate made from ferrous sulfate and industrial sulfuric acid, a by-product of titanium dioxide production through the sulfuric acid process. This product is mainly used as a water purifier.
Molecular formula: [Fe2(OH),(SO4)-..
2 reference standards
GB190
G3191
G3 602
GB 602
GB603
Dangerous goods packaging markings| |tt||Packaging, storage and transportation pictorial mark
Preparation of standard solution for chemical reagent titration analysis (volume analysis) Preparation of standard solution for impurity determination
Chemical reagent
Chemical reagent test Preparation of preparations and products used in the method GB 610.2 | | tt | | GB1250 | | tt | /T 6678
General principles for sampling of chemical products
Analytical laboratory water specifications and test methods GB66821
Plastic woven bags
GB8946
3 product classifications|| tt||Polymerized ferric sulfate products are divided into type I and phenanthrene type according to their status. Type I is liquid and type I is solid. 4 Technical requirements
4.1 Appearance: It is a reddish-brown viscous transparent liquid; it is a light yellow amorphous solid. 4.2 Sulfur iron shall comply with the requirements of Table 1.
National Technical Supervision Bureau 7993-08-06 approved implementation on 1994-09-01
61
item
Xie degree/cm(2nC)||tt| |Gold and iron content, is
mesh
containing reducing substances (calculated as Fer+), %
drum base,
H (1*aqueous solution)| | tt | |tt||Table 1
Type
1,45
11.0
0.10
9.0-14.0
2.03.0|| tt||0.0005
0.0010
0.3
93
refers
standard
type
18.5||tt| |0.15
9.0~14, 0
2.0~3.0
0.0008
0.0015
0.5
In the test piece method, except for special Unless otherwise specified, only analytically pure reagents and grade 3 water complying with CB6682 should be used. Standard solutions, preparations and products required in the test: Unless other regulations are noted, they shall be prepared in accordance with the regulations of GB601, GB602.GB603.
5. Determination of density (densitometer method)
5.1.1 Method summary
Use the depth of immersion of the density meter when it reaches equilibrium in the liquid to be measured to read the density. Density of liquid. 5.1.2 Instruments and equipment
5.1.2.1 Density: the scale value is 0.001g/cm; 5.1.2.2 Constant temperature water bath: the temperature can be controlled to 20±1C; 5.1.2.3 Thermometer: the scale value is 1℃: 5.1.2.4 Cylinder: 250~~500ml*
5.1.3 Measurement steps
Inject the polyferric sulfate sample (Type I) into a clean and dry measuring cylinder without any bubbles. Place the measuring stick in a constant temperature water bath at 20±1C! , wait until the temperature becomes constant, slowly place the density meter into the sample, and after the density meter is stable in the sample, read the scale on the lower edge of the meniscus of the density meter (marked with the scale on the upper edge of the meniscus) Densitometer is excluded), which is the density of the sample at 20°C. 5.2 Determination of total iron content
5.2.1 Potassium dichromate method
5.2.1.1 Method summary
In acidic solution, use oxide to reduce ferric iron to divalent iron Iron, excess stannous chloride is removed with mercury oxide, and then titrated with a standard titration solution of potassium dichromate.
The technical equation is:
2Fe| +Sn21 2Fe2++Sn++
SnCI+ 2HgC1-SnCI +Hg.C12
6Fet +Cr0F +14Ht 6Fe*++ 2Cr3+ +7H205.2.1.2 Reagents and materials
a. Continental tin chloride (GB638): 250g/L solution; weigh 25.0g stannous chloride into a dry beaker, dissolve in 20mL hydrochloric acid, After cooling, dilute to 100ml and store in a brown dropper bottle. Add a few high-purity tin particles.
62
Hot acid (GB622): 1+1 solution;
Good, 3
Mercuric chloride (HG3-1068): saturated solution; c.| | tt | tt||Potassium dichromate (GB642) standard titration solution: ℃e.
f, sodium diphenylamine sulfonate solution 5 milliliter/L.
K,Cr.O
0, 1 mol/L
5.2.1.3 Analysis steps
Type 1 product Weigh about 1.5g sample, Type 1 product Weigh about 0.9g of the sample, accurate to 0.001g+, and place it in a 250m Erlenmeyer flask: add 20ml of water, add 20ml of hydrochloric acid solution (5.2.1.2b), heat to boiling, add stannous chloride solution (5.2.1.2) thermotically. a) Until the yellow color of the solution disappears, add another 1 drop, cool quickly, add 5 ml of mercuric chloride solution (5.2.1.2c), shake well and let it stand for 1 minute, then add 50 mL of water, and add sulfur-phosphorus mixed acid (5.2.1.2 d) 10mL, add 4-~5 drops of sodium diphenylamine sulfonate indicator solution (5.2.1.2f), and titrate with potassium dichromate standard titration solution (5.2.1.2e) until purple (not fading in 30s) is the end point. 5.2.1.4 Expression of analysis results
Total iron content X expressed as mass percentage, calculated according to formula (1): ||In the formula: the volume of the potassium dichromate standard titration solution consumed by the sample at the stoichiometric point is the concentration of the potassium dichromate standard titration solution mol/L and the mass of the sample,
0.05585- and 1.00 mL potassium dichromate standard titration solution c the mass of iron.
5.2.2 Titanium trichloride method
(1)
K, Cr.O, =1.000mol/L1 equivalent, expressed in grams 5.2.2.1 Method summary| |tt||In the acidic solution, titanium trichloride solution is added dropwise to reduce the ferric ions to divalent iron ions. The excess titanium trinitride further reduces the sodium tungstate indicator solution to produce "blue", making the solution blue. . Under the catalysis of copper salt, the excess titanium trichloride is oxidized by the dissolved oxygen in the water. After the blue color of the solution disappears, use sodium diphenylamine sulfonate as the indicator solution and titrate with potassium dichromate standard titration solution. . The reaction equation is:
Fe3i -→+ Tiat -Fe2+ +Tis-t
6Fe2+CrO+14Ht 6Feat +2Cr3++7H,05.2.2.2 Reagents and materials
a.
h.
c.
Hydrochloric acid (GB622) solution: 1+1;
Sulfuric acid (GB625) solution: 1+1;
Phosphoric acid (GB1282) solution: 15+85
Copper sulfate (GB665) solution: 5g/L
Titanium difluoride solution: Measure 25mL of 15% titanium trifluoride solution and add 20mL of hydrochloric acid (GB622 ), dilute with water to e
100mL, mix well, and store in a brown bottle. Add a thin layer of liquid paraffin to protect the solution. It can be used for about 15 days; f. Sodium tungstate solution: 25g/L. Weigh 2.Dissolve 5g sodium tungstate in 70mL water, add 7mL phosphoric acid (CB1282), cool and dilute to 100mL with water, mix and store in a brown bottle: c(IK,Cr20.) 0. 015 mol/L;||tt ||g, potassium dichromate (GB642) standard titration solution: ch. Sodium diphenylamine sulfonate (same as 5.2.1.2f). 5.2.2.3 Analysis steps
Weigh about 0.2~~0.3g sample to the nearest 0.0001g, place it in a 250ml Erlenmeyer flask, add 10ml of hydrochloric acid solution (5.2.2.2a), 63||tt| |GB14591-93
10mL of sulfuric acid solution (5.2.2.2b) and 1m of sodium tungstate indicator solution (5.2.2.2f). With constant shaking, add titanium trifluoride solution (5.2.2.2c) dropwise until the solution just appears blue. Rinse the inner wall of the Erlenmeyer flask with water and dilute it to about 150mL. Add 2 drops of copper sulfate solution (5.2.2.2d). Shake it thoroughly. After the blue color of the solution disappears, add 10mL and 2 drops of phosphoric acid solution (5.2.2.2c). Sodium dipyridine sulfonate indicator solution (5.2.2.2h), immediately titrate with potassium dichromate standard titration solution (5.2.2.2g) until purple (does not fade for 30s) is the end point, 5.2.2.4 Expression of analysis results | |tt|| Total iron content The volume of potassium dichromate standard titration solution consumed by the sample, mL.—the concentration of potassium dichromate standard titration solution mo1/L; m—the mass of the sample, g;
0.05585—and 1.00 mL potassium dichromate standard titration solution c the base of iron.
.(2)
-K, Cr, 0, =1.000nol/L equivalent, expressed in grams =
5.2.3 Allowable difference
Take the arithmetic mean of the parallel measurement results as the measurement result, and the absolute difference between the two parallel measurement results shall not be greater than 0.1%. The absolute difference in the measurement results of different test plugs is not greater than 0.15%. 5.3 Determination of the content of reducing substances (calculated as Fe2+) 5.3.1 Method summary
Titrate with potassium permanganate standard titration solution in acidic solution. The reaction equation is:
Mn0, +5Fe2 +8H+Mn*t+5Fe+-→4H05.3.2 Reagents and materials
5.3.2.1 Sulfuric acid (GB625);
5.3.2.2 Phosphoric acid (GB1282)
(green KMno.) =0.1 mol/L:
5.3.2.3 Potassium permanganate (GB643) standard titration solution: C15
5.3.2.4 High manganese Potassium permanganate standard titration solution: Dilute the potassium permanganate standard titration solution in 5.3.2.3 10 times, prepare it as you go, and use it on the same day.
5.3.3 Instruments and equipment
5.3.3.1 Microburette: 1mlL.
5.3.4 Analysis steps
Weigh about 5g sample, accurate to 0.001g, place it in a 250mL Erlenmeyer flask, add 50ml of water, 4mL of sulfuric acid (5.3.2.1), phosphoric acid (5.3 .2.2) 4ml shake hook. Use potassium permanganate standard titration solution (5.3.2.4) to titrate to a light red color (not fading for 30 seconds) which is the end point, and perform a short self-test at the same time.
5.3.5 Expression of analysis results
The content of reducing substances (calculated as Fez+) expressed as mass percentage X. Calculate according to formula (3): 2.4), mLV, - the volume of the permanganate standard titration solution (5.3.2.4) consumed by the blank at the stoichiometric point, ml. - the concentration of the potassium permanganate standard titration solution (5.3.2.4), mo1 /L1(3)
#—The mass of the sample, g:
0.05585-equivalent to 1.00ml potassium permanganate standard titration solution [cl-KMnO] 1.000mol/L, expressed in grams Represents the quality of 6-
iron.
5.3.6 Allowable difference
GB14591-93
Take the arithmetic mean of the parallel measurement results as the measurement result. The absolute difference between the two parallel measurement results shall not be greater than 0.01%: The absolute difference between the measurement results of different laboratories is not greater than 0.015%. 5.4 Determination of salinity
5.4.1 Method summary
Add a certain amount of hydrochloric acid solution to the sample, then mask the iron with potassium fluoride, and then titrate with the sodium oxyhydroxide standard titration solution. 5.4.2 Reagents and materials
5.4.2.1 Hydrochloric acid (GB622) solution: 1+35.4.2.2 Sodium hydroxide (GB629) solution: c (NaOH)㎡=0.1mol/L5.4.2.3 Hydrochloric acid (GB 622) Solution: c (HC1)=0.1 mol/L5.4.2.4 Potassium fluoride (GB1271) solution: 500g/L. Weigh 500g of potassium fluoride, dissolve it in 200mL of distilled water without carbon dioxide, dilute to 1000mL, add 2mL of phenolic acid indicator and adjust the solution to Reddish in color, filter out insoluble matter and store in plastic bottles. 5.4.2.5 Sodium hydroxide (GB629) standard titration solution: (NaOH) = 0.1mol/L; 5.4.2.6 Phenol (GB10729) ethanol solution: 10g/15.4.3 Analysis steps
Weigh about 1.5g The sample, accurate to 0.001g, is placed in a 250mL Erlenmeyer flask, accurately adds 25.00ml hydrochloric acid solution (5.4.2.3) with a pipette, adds 20mL boiled and cooled distilled water, shakes, and covers the surface. Leave it at room temperature for 10 minutes, then add 10ml of potassium fluoride solution (5.4.2.4), shake well and add 5 drops of phenolic indicator (5.4.2.6), and immediately titrate with sodium hydroxide standard titration solution (5.4.2.5) To talk about red (303 does not fade) is the end point. At the same time, use boiled and cooled distilled water instead of the sample to do a blank test. 5.4.4 Analysis of the expression of nesting
Balinity |tt||X
mx
18.62
~ × 100
(V. V) : c |tt||mx
Where: the volume of the sodium hydroxide standard titration solution consumed by the blank test at the stoichiometric point, the volume of the sodium hydroxide standard titration solution consumed by the sample at the mLV stoichiometric point ,.-concentration of sodium hydroxide standard titration solution·mo1/L; m-mass of the sample, g:
X,--mass percentage of ferric iron in the sample, X= X, tt||18.62-Molar mass of iron M
IFe
+g/rmol
5.4.5 Allowable difference
Take the arithmetic mean of the parallel measurement results as the determination As a result, the absolute difference between the two parallel measurement results was no more than 0.2%. The absolute difference between the measurement results of different laboratories shall not be greater than 0.5%. 5.5 Determination of pH value
5.5.1 Reagents and materials
5.5.1.1 Potassium hydrogen phthalate buffer solution with pH 4.00; 65
GB 14591—93||tt ||5.5.1.2 Potassium dihydrogen phosphate-potassium hydrogen phthalate buffer solution with pH~6.86. 5.5.2 Instruments and equipment
5.5.2.1 Acidometer: accuracy 0.1pH;
5.5.2.2 glass electrode;
5.5.2.3 saturated calomel electrode;
5.5.3 Measurement steps
5.5.3.1 Preparation of sample solution
Weigh 1.0g of the sample, place it in a beaker, dilute it with water, transfer it all to a 100ml volumetric flask and dilute it to the mark. Shake the hook. 5.5.3.2 Determine
using potassium hydrogen phthalate buffer solution with pH=4.00 and pH=6.86 potassium dihydrogen phosphate-potassium hydrogen phthalate buffer solution, pour the sample solution (5.5.3.1) into the beaker, immerse the saturated calomel electrode and glass electrode into the solution to be measured, until the pH value stabilizes (The change in pH value within 1 minute is not greater than 0.1) reading. 5.6 Determination of insoluble matter content
5.6.1 Reagents and materials
5.6.1.1 Hydrochloric acid ((GB622) solution: 1+49. 5.6.2 Instruments and equipment
5.6. 2.1 Electric constant temperature drying oven: the temperature can be controlled at 105~110℃; 5.6.2.2 type filter
5.6.3 Analysis steps
Weigh approximately in a dry and clean weighing bottle. 20g of type 1 sample, or 10g of type 1 sample, accurate to 0.001g, is transferred into a 250mL beaker. For type 1 sample, wash the weighing bottle with water several times, add the washing liquid into the beaker containing the sample, and add water to approximately 100mL. Stir the Type I sample evenly, wash the weighing bottle with hydrochloric acid solution (5.6.1.1) in batches, put the washing liquid into the beaker holding the sample, add hydrochloric acid solution (5.6.1.1) to a total volume of about 100ml. Stir to dissolve and keep in a 50±5°C water bath for 15 minutes. Filter with a crucible filter that has been dried at 105~110°C to constant weight. Wash the residue with water until the filtrate does not contain chloride ions (check with silver nitrate solution). Put the sweet worm into an electric constant temperature drying oven and bake it at 105-110°C until it reaches constant weight.
5.6.4 Expression of analysis results
Insoluble matter content X expressed as mass percentage. According to the formula 5) Calculation: tt||Quality of sample·8.
5.7 Determination of arsenic content
Silver diethyldithiocarbamate photometric method (5)
5.7.1 Method summary
The arsenide in the sample is reduced to trivalent arsenic under the action of potassium arsenide and acidic stannous chloride. The new ecological oxygen generated by the interaction of trivalent arsenic with zinc and acid generates arsine hydrogen gas, which passes through acetic acid. The lead-soaked cotton is used to remove the interference of hydrogen sulfide, and then reacted with silver diethyldithiocarbamate to form a brown red envelope colloidal solution, and the absorbance is measured at 530nm. 5.7.2 Reagents and materials
5.7.2 , 1 Sulfuric acid (GB625) solution: 1+9; 5.7.2.2 Sulfuric acid (GB625) solution: 1+1; 5.7.2.3 Sodium hydroxide (GB629) solution: 100g/L, 5.7.2.4 Stannous fluoride (GB638) Hydrochloric acid solution: 400g/1. Weigh 4g of stannous chloride (SnCl2·2HzO) and add 10ml of hydrochloric acid (GB622). Dissolve, dilute to 100ml with water, add a few metal tin particles, and store in a brown reagent bottle; G | | tt | ·Put 3H207 in 100mL water and add J drops of Z acid solution (CH.OOOH) = 6mol/.: 5.7.2.7 Lead acetate cotton: Take skimmed cotton and soak it in lead acetate solution (5.7.2.6) for 2 hours, then drain it. Dry naturally or bake in a 100°C oven and store in a dry and dense bottle:
5.7.2.8 Silver Ethyldithiocarbamate Triethanolamine Trichloromethane Solution (hereinafter referred to as the absorption solution): weigh 0.25 g of silver diethyldithiocarbamate, dissolve it with a small amount of chloroform, add 2 ml of triethanolamine, dilute 100 mL with trifluoromethane, let it sit overnight, filter it into a brown bottle, and place it in the refrigerator at 4°C Preservation; 5.7.2.9 Arsenic standard stock solution: Accurately weigh 0.1320g of dioxide which has been dried in sulfuric acid to a heavy weight, warmly dissolve it in 1.2ml of sodium oxide solution (5.7.2.3), and transfer In a 1000mL volumetric flask, dilute to the mark. This stock solution contains 0.1mglt
per 1ml. 5.7.2.10 Crushed standard solution: Take 10mL of the standard stock solution into a 100mL container, add 1mL of sulfuric acid solution (5.7.2.1): Add water to dilute to the mark. , mixed sentences. Before use, take 10 mL of this solution and place it in a 100 mL volumetric flask. Add water to dilute to the mark. 1 ml of this solution contains 0.001 mg arsenic.
5.7.3 Instruments and equipment
5.7.3.1 Stabilizer: See Article 5.3 of GB610.2: 5.7.3.2 Spectrophotometer:
5.7.4 Analysis steps| |tt||5.7.4.1 Accurately weigh 1.000g of Type 1 sample or 0.600g of Type 1 sample + accurate to 0.0002g + and put it into the conical flask of the stele-fixing device, and put it in the conical flask of another stele-fixing device. Accurately put in 5.00mL of stele standard solution, add 3mL of sulfuric acid solution (5.7.2.2) respectively, and after discharging to 30mL with water, add 2mL of potassium iodide solution (150/L) and let stand for 2~3 minutes, and stannous chloride solution (5.7 .2.4) 1.0mL, mix 5. Leave for 15 min.
5.7.4.2 Add 5.0mL of absorption solution (5.7.2.8) into the graduated absorption tubes, and insert cotton with lead acetate (5.7. 2.7) into the trachea, quickly pour 5g of pre-measured arsenic-free zinc particles (5.7.2.5) into the generating bottle, and immediately plug the bottle stopper to prevent air leakage. React at room temperature for 1 hour. Finally, use trioxane to replenish the volume of the absorbent solution to 5.0 mL. Within 1 hour, use a 1.0 cm absorption cell to measure the absorbance of the sample and standard solution at a wavelength of 530 nm. If the absorbance of the sample is lower than the absorbance of the standard solution, it meets the standard. Meanwhile, tune the instrument using the reagent blank. 5.8 Determination of lead content
5.8.1 Disulfide photometric method
5.8.1.1 Method summary
Use ammonia to adjust the pH to 8.5~9.0, and add potassium cyanide for masking agent, use disulfide chloroform extraction and nitrate extraction to remove interfering ions, and finally form a brick red complex with disulfide gland, and then measure its absorbance. 5.8.1.2 Reagents and materials
Lead-free distilled water is required for preparing reagents and diluting water. &, Lead-free distilled water: Pass the water through a cation exchange resin to remove lead from the water: Lead standard recommendation solution: Weigh 0.1598g of lead nitrate CPb (NO.) 23 baked at 110C and dissolve it into water containing 1 mL of concentrated nitric acid. (5.8.1.2a), and dilute to 1000ml with water (5.8.1.2a). 1.00ml of this solution contains 0.100m lead; c. Lead standard solution: draw 10.00ml of lead standard stock solution, and use water (5.8.1.2a) ) diluted to 500mL, 1ml of this solution contains 0.002mg lead. Current use:
d． Phenol red (HG3-959) indicator solution: 1.0g/1. Ethanol solution, weigh 0.1g of phenol red and dissolve it in 100ml.95% ethanol e. Disulfon-trimethane preparation solution: 0.1% solution is prepared according to Appendix A; 1. Disulfide-trifluoromethane solution with an absorbance of 0.15: Take an appropriate amount of disulfide-trifluoromethane stock solution and dilute it with chloroform to The absorbance is 0.15 wavelength 510nm + 1zm colorimetric m), currently used and equipped: 67
GB 14591-93
g. Ammonium citrate solution: 50% solution, prepared according to Appendix B; h. Hydroxylamine hydrochloride solution: 200g/L. Weigh 20g of hydroxylamine hydrochloride (NH2OH·HC1), dissolve it in water (5.8.1.2a), and dilute to 100ml. Purify according to Appendix C;
i. Potassium rat solution: 100g/L. Weigh 10g of potassium cyanide (KCN), dissolve it in water (5.8.1.2a), and dilute to 100ml. Note: Potassium fluoride is a highly toxic substance.
Ammonia (GB631) solution: 1+1
j.
k. Nitric acid (GB626) solution: 3+97;
1. Nitric acid (GB626) solution: 1+9;
m, chloroform (GB682);
nitric acid (GB626).
n.
5.8.1.3 Instruments and equipment
All glass instruments need to be soaked in nitric acid solution (5.8.1.21) overnight, and then washed with water. Separating funnel: 125mL,
a,
graduated colorimetric tube: 10mL, with stopper:
b.
spectrophotometer.
c.
5.8.1.4 Analysis steps
a. Weigh 1.0g of Type I sample or 0.6g of Type I sample, accurate to 0.001g, put it into a 200mL beaker, add 50mL of water, nitric acid (5.8.1.2n) Boil 1.0mL on an electric stove for 3 minutes. After cooling, put it into a 100mL volumetric flask, add water (5.8.1.2a), and dilute to the mark.
b． Accurately draw 50.00mL of the above solution into the first separatory funnel (5.8.1.3a), add 10.0ml of ammonium citrate solution (5.8.1.2g), 10.0mL of hydroxylamine hydrochloride solution (5.8.1.2h), and phenol red indication 3 drops of solution (5.8.1.2d), shake well, adjust the pH to -8.5~9.0 with nitrogen aqueous solution (5.8.2.1i), add 4.0mL of potassium cyanide solution (5.8.1.2i), shake well, add double 10.0 ml of sulfur chloroform solution 5.8.1.2f), shake for 1 min, and let stand to separate layers; put the chloroform layer into the second separatory funnel, and then add 10.0 mL to the first separatory funnel. .The disulfide-trichloromethane solution (5.8.1.2f) was shaken for 1 minute, allowed to stand and separated into layers. The chloroform layer was then merged into the second separatory funnel-1, and 30.0 mL was added to the second separatory funnel. Shake the nitric acid solution (5.8.1.2k) for 1 minute, let stand and separate into layers, discard the chloroform layer, add 20 mL of water (5.8.1.2a), shake, and add 10.0 mL of ammonium citrate solution (5.8.1.2g). 10.0ml of hydroxylamine hydrochloride solution (5.8.1.2h), 1 drop of phenol red indicator solution (5.8.1.2d), spread evenly, add 2.0mL of ammonia solution (5.8.1.2f), add potassium cyanide solution (5.8.1.21 )1.0mL, shake well; add 10.0mL of disulfonate chloroform solution (5.8.1.2f), shake for 1 minute, let stand for stratification, put a small amount of absorbent cotton into the neck of the separation funnel, and place the chloroform layer Put it into a dry colorimetric tube and dilute it to the mark with disulfide adenotrichloromethane solution (5.8.1.2f) with an absorbance of 0.15.
Take another separatory funnel (5.8.1.3a), add 2.5mL of lead standard solution (5.8.1.2c), and add ammonium citrate solution.
(5.8.1.2g) 10.0ml., 2.0mL of hydroxylamine hydrochloride solution (5.8.1.2h), 1 drop of phenol red indicator solution (5.8.1.2d), shake, adjust to pH 8.5~9.0 with ammonia solution (5.8.1.2j), add Potassium cyanide solution (5.8.1.2i) 4.0 mL, shake well. Add 10.0 ml of disulfide chloroform solution (5.8.1.2f), shake for 1 minute, and let stand for layering; stuff a small amount of absorbent cotton into the neck of the separatory funnel, and put the chloroform layer into a dry colorimetric tube (5.8 .1.3b), dilute to the mark with trifluoromethane solution (5.8.1.2f) with an absorbance of 0.15. d. At a wavelength of 510nm, use a 1.0cm absorption cell, adjust the zero point with disulfide chloroform solution (5.8.1.2f), and measure the absorbance of the sample and standard sample. If the absorbance of the sample is lower than the absorbance of the standard sample, it meets the standard. The test cyanide-containing waste liquid shall be treated according to Appendix E before being discharged. 5.8.2 Atomic absorption spectrometry (arbitration method) 5.8.2.1 Method summary
Add nitric acid and hydrogen peroxide to the sample to dissolve the lead in the sample, and then use atomic absorption spectrometry to determine the lead content. 5.8.2.2 Reagents and materials
a. Nitric acid (GB626) solution: excellent grade pure, 1+1; b. Nitric acid (GB626) solution: excellent grade pure, 1+199; 68
t． Chlorine peroxide (GB684): superior grade pure; GB 1459193
d． Lead standard solution: 1mL solution contains 0.1mgPb, prepared according to GB602;
Lead standard solution: 1mL. The solution contains 0.0010mgPb. Use a pipette to transfer 5.0mL of lead standard solution (5.8.2.2d) into a 500ml volumetric flask, add nitric acid solution (5.8.2.2h) to the mark, and shake well. This solution is ready for use. 5.8.2.3 Instruments and equipment
The glass instruments used must be cleaned with nitric acid solution (5.8.2.2a) and then with water (5.8.1.2a). a. Fluorine gas cylinder;
, atomic absorption spectrometer: equipped with graphite furnace control device, lead hollow cathode lamp, ambient lamp or Zeeman background subtraction device, 200L micro-quantitative sampler.
Refer to Table 2 for atomization parameters.
Dry
Content C
Ramp up.s
Maintenance: 5
Argon flow salt+ml./min
5.8 .2.4 Analysis steps
200
20
10
300
FE
table?
ashing
600
1o
20
300
atomization
2300
1
5
50
Delete
2500
1
2
300
a, Drawing of working curve
Use a pipette to pipette 0.0, 1.0.3.0, 5.0.7.0, 9.0mL lead standard solution (5.8.2.2e) respectively, place it in six 100mL volumetric flasks, and add nitric acid solution (5.8.2.2b) to the mark and spread evenly. According to the instrument manual, adjust the various conditions of the atomic absorption spectrometer to the optimal state. After zeroing with a reagent blank, measure the absorbance of each standard solution separately. Draw a working curve with the lead content as the abscissa and the corresponding absorbance as the ordinate. b Determination
Weigh about 3g of the sample, accurate to 0.01g, transfer it to a 1000mL volumetric flask, add water to dilute to the mark, and shake the hook. Use a pipette to accurately transfer 50.00mL of the above solution, place it in a 250mL beaker, add water to 100mLL, carefully add 2.0mL hydrogen peroxide (5.8.2.2c) and 2.0mL nitric acid solution (5.8.2.2a), and heat Evaporate until the volume of the solution is approximately 40 mL, cool to room temperature, completely transfer the solution to a 100 mL volumetric flask, add water to the mark, and shake well. Use the same working conditions as those used to measure the standard solution to measure its absorbance, and do a reagent blank test at the same time.
5.8.2. Expression of analysis results
The lead content (X,) expressed as a percentage of the amount is calculated according to formula (6): 2(m- no)
X 100| |tt||X,
m The absorbance of the reagent blank solution, the mass of lead detected from the working curve, m the mass of the sample·.
t5
5.8.2.6 Allowable difference
Take the arithmetic mean of the parallel measurement results as the measurement result. The absolute difference between the two parallel measurement results shall not be greater than 0.0003%. 6 Inspection Rules
6.1 Polyferric sulfate shall be inspected for product quality by the quality inspection department of the manufacturer in accordance with the test methods and inspection rules specified in this standard. The manufacturer shall ensure that all products shipped meet the requirements of this standard. . 6.2 Each batch of products leaving the factory should be accompanied by a quality instruction sheet, including: manufacturer name, product name, grade, batch number, production date, net 69
1.2f) 2.0 mL, add 1.0 mL of potassium cyanide solution (5.8.1.21), shake well; add 10.0 mL of disulfonate chloroform solution (5.8.1.2f), shake for 1 min, let stand and separate. Put a small amount of absorbent cotton into the neck of the liquid funnel, put the chloroform layer into a dry colorimetric tube, and dilute it to the mark with a disulfide chloroform solution (5.8.1.2f) with an absorbance of 0.15.
Take another separatory funnel (5.8.1.3a), add 2.5mL of lead standard solution (5.8.1.2c), and add ammonium citrate solution.
(5.8.1.2g) 10.0ml., 2.0mL of hydroxylamine hydrochloride solution (5.8.1.2h), 1 drop of phenol red indicator solution (5.8.1.2d), shake, adjust to pH 8.5~9.0 with ammonia solution (5.8.1.2j), add Potassium cyanide solution (5.8.1.2i) 4.0 mL, shake well. Add 10.0 ml of disulfide chloroform solution (5.8.1.2f), shake for 1 minute, and let stand for layering; stuff a small amount of absorbent cotton into the neck of the separatory funnel, and put the chloroform layer into a dry colorimetric tube (5.8 .1.3b), dilute to the mark with trifluoromethane solution (5.8.1.2f) with an absorbance of 0.15. d. At a wavelength of 510nm, use a 1.0cm absorption cell, adjust the zero point with disulfide chloroform solution (5.8.1.2f), and measure the absorbance of the sample and standard sample. If the absorbance of the sample is lower than the absorbance of the standard sample, it meets the standard. The test cyanide-containing waste liquid shall be treated according to Appendix E before being discharged. 5.8.2 Atomic absorption spectrometry (arbitration method) 5.8.2.1 Method summary
Add nitric acid and hydrogen peroxide to the sample to dissolve the lead in the sample, and then use atomic absorption spectrometry to determine the lead content. 5.8.2.2 Reagents and materials
a. Nitric acid (GB626) solution: excellent grade pure, 1+1; b. Nitric acid (GB626) solution: excellent grade pure, 1+199; 68
t． Chlorine peroxide (GB684): superior grade pure; GB 1459193
d． Lead standard solution: 1mL solution contains 0.1mgPb, prepared according to GB602;
Lead standard solution: 1mL. The solution contains 0.0010mgPb. Use a pipette to transfer 5.0mL of lead standard solution (5.8.2.2d) into a 500ml volumetric flask, add nitric acid solution (5.8.2.2h) to the mark, and shake well. This solution is ready for use. 5.8.2.3 Instruments and equipment
The glass instruments used must be cleaned with nitric acid solution (5.8.2.2a) and then with water (5.8.1.2a). a. Fluorine gas cylinder;
, atomic absorption spectrometer: equipped with graphite furnace control device, lead hollow cathode lamp, ambient lamp or Zeeman background subtraction device, 200L micro-quantitative sampler.
Refer to Table 2 for atomization parameters.
Dry
Content C
Ramp up.s
Maintenance: 5
Argon flow salt+ml./min
5.8 .2.4 Analysis steps
200
20
10
300
FE
table?
ashing
600
1o
20
300
atomization
2300
1
5
50
Delete
2500
1
2
300
a, Drawing of working curve
Use pipettes to pipette 0.0, 1.0.3.0, 5.0.7.0, 9.0mL lead standard solutions (5.8.2.2e) respectively, place them in six 100mL volumetric flasks, and add nitric acid solution (5.8.2.2b) to the mark and spread evenly. According to the instrument manual, adjust the various conditions of the atomic absorption spectrometer to the optimal state. After zeroing with a reagent blank, measure the absorbance of each standard solution separately. Draw a working curve with the lead content as the abscissa and the corresponding absorbance as the ordinate. b Determination
Weigh about 3g of the sample, accurate to 0.01g, transfer it to a 1000mL volumetric flask, add water to dilute to the mark, and shake the hook. Use a pipette to accurately transfer 50.00mL of the above solution, place it in a 250mL beaker, add water to 100mL, carefully add 2.0mL hydrogen peroxide (5.8.2.2c) and 2.0mL nitric acid solution (5.8.2.2a), and heat Evaporate until the volume of the solution is approximately 40 mL, cool to room temperature, completely transfer the solution to a 100 mL volumetric flask, add water to the mark, and shake well. Use the same working conditions as those used to measure the standard solution to measure its absorbance, and do a reagent blank test at the same time.
5.8.2. Expression of analysis results
The lead content (X,) expressed as a percentage of the amount is calculated according to formula (6): 2(m- no)
X 100| |tt||X,
m The absorbance of the reagent blank solution, the mass of lead detected from the working curve, m the mass of the sample·.
t5
5.8.2.6 Allowable difference
Take the arithmetic mean of the parallel measurement results as the measurement result. The absolute difference between the two parallel measurement results shall not be greater than 0.0003%. 6 Inspection Rules
6.1 Polyferric sulfate shall be inspected for product quality by the quality inspection department of the manufacturer in accordance with the test methods and inspection rules specified in this standard. The manufacturer shall ensure that all products shipped meet the requirements of this standard. . 6.2 Each batch of products leaving the factory should be accompanied by a quality instruction sheet, including: manufacturer name, product name, grade, batch number, production date, net 69
1.2f) 2.0 mL, add 1.0 mL of potassium cyanide solution (5.8.1.21), shake well; add 10.0 mL of disulfonate chloroform solution (5.8.1.2f), shake for 1 min, let stand and separate. Put a small amount of absorbent cotton into the neck of the liquid funnel, put the chloroform layer into a dry colorimetric tube, and dilute it to the mark with a disulfide chloroform solution (5.8.1.2f) with an absorbance of 0.15.
Take another separatory funnel (5.8.1.3a), add 2.5mL of lead standard solution (5.8.1.2c), and add ammonium citrate solution.
(5.8.1.2g) 10.0ml., 2.0mL of hydroxylamine hydrochloride solution (5.8.1.2h), 1 drop of phenol red indicator solution (5.8.1.2d), shake, adjust to pH 8.5~9.0 with ammonia solution (5.8.1.2j), add Potassium cyanide solution (5.8.1.2i) 4.0 mL, shake well. Add 10.0 ml of disulfide chloroform solution (5.8.1.2f), shake for 1 minute, and let stand for layering; stuff a small amount of absorbent cotton into the neck of the separatory funnel, and put the chloroform layer into a dry colorimetric tube (5.8 .1.3b), dilute to the mark with trifluoromethane solution (5.8.1.2f) with an absorbance of 0.15. d. At a wavelength of 510nm, use a 1.0cm absorption cell, adjust the zero point with disulfide chloroform solution (5.8.1.2f), and measure the absorbance of the sample and standard sample. If the absorbance of the sample is lower than the absorbance of the standard sample, it meets the standard. The test cyanide-containing waste liquid shall be treated according to Appendix E before being discharged. 5.8.2 Atomic absorption spectrometry (arbitration method) 5.8.2.1 Method summary
Add nitric acid and hydrogen peroxide to the sample to dissolve the lead in the sample, and then use atomic absorption spectrometry to determine the lead content. 5.8.2.2 Reagents and materials
a. Nitric acid (GB626) solution: excellent grade pure, 1+1; b. Nitric acid (GB626) solution: excellent grade pure, 1+199; 68
t． Chlorine peroxide (GB684): superior grade pure; GB 1459193
d． Lead standard solution: 1mL solution contains 0.1mgPb, prepared according to GB602;
Lead standard solution: 1mL. The solution contains 0.0010mgPb. Use a pipette to transfer 5.0mL of lead standard solution (5.8.2.2d) into a 500ml volumetric flask, add nitric acid solution (5.8.2.2h) to the mark, and shake well. This solution is ready for use. 5.8.2.3 Instruments and equipment
The glass instruments used must be cleaned with nitric acid solution (5.8.2.2a) and then with water (5.8.1.2a). a. Fluorine gas cylinder;
, atomic absorption spectrometer: equipped with graphite furnace control device, lead hollow cathode lamp, ambient lamp or Zeeman background subtraction device, 200L micro-quantitative sampler.
Refer to Table 2 for atomization parameters.
Dry
Content C
Ramp up.s
Maintenance: 5
Argon flow salt+ml./min
5.8 .2.4 Analysis steps
200
20
10
300
FE
table?
ashing
600
1o
20
300
atomization
2300
1
5
50
Delete
2500
1
2
300
a, Drawing of working curve
Use pipettes to pipette 0.0, 1.0.3.0, 5.0.7.0, 9.0mL lead standard solutions (5.8.2.2e) respectively, place them in six 100mL volumetric flasks, and add nitric acid solution (5.8.2.2b) to the mark and spread evenly. According to the instrument manual, adjust the various conditions of the atomic absorption spectrometer to the optimal state. After zeroing with a reagent blank, measure the absorbance of each standard solution separately. Draw a working curve with the lead content as the abscissa and the corresponding absorbance as the ordinate. b Determination
Weigh about 3g of the sample, accurate to 0.01g, transfer it to a 1000mL volumetric flask, add water to dilute to the mark, and shake the hook. Use a pipette to accurately transfer 50.00mL of the above solution, place it in a 250mL beaker, add water to 100mL, carefully add 2.0mL hydrogen peroxide (5.8.2.2c) and 2.0mL nitric acid solution (5.8.2.2a), and heat Evaporate until the volume of the solution is approximately 40 mL, cool to room temperature, completely transfer the solution to a 100 mL volumetric flask, add water to the mark, and shake well. Use the same working conditions as those used to measure the standard solution to measure its absorbance, and do a reagent blank test at the same time.
5.8.2. Expression of analysis results
The lead content (X,) expressed as a percentage of the amount is calculated according to formula (6): 2(m- no)
X 100| |tt||X,
m The absorbance of the reagent blank solution, the mass of lead detected from the working curve, m the mass of the sample·.
t5
5.8.2.6 Allowable difference
Take the arithmetic mean of the parallel measurement results as the measurement result. The absolute difference between the two parallel measurement results shall not be greater than 0.0003%. 6 Inspection Rules
6.1 Polyferric sulfate shall be inspected for product quality by the quality inspection department of the manufacturer in accordance with the test methods and inspection rules specified in this standard. The manufacturer shall ensure that all products shipped meet the requirements of this standard. . 6.2 Each batch of products leaving the factory should be accompanied by a quality instruction sheet, including: manufacturer name, product name, grade, batch number, production date, net 69
s
Hold: 5
Argon flow salt+ml./min
5.8.2.4 Analysis steps
200
20
10
300
FE
table?
ashing
600
1o
20
300
atomization
2300
1
5
50
Delete
2500
1
2www.bzxz.net
300
a, Drawing of working curve
Use pipettes to pipette 0.0, 1.0.3.0, 5.0.7.0, 9.0mL lead standard solutions (5.8.2.2e) respectively, place them in six 100mL volumetric flasks, and add nitric acid solution (5.8.2.2b) to the mark and spread evenly. According to the instrument manual, adjust the various conditions of the atomic absorption spectrometer to the optimal state. After zeroing with a reagent blank, measure the absorbance of each standard solution separately. Draw a working curve with the lead content as the abscissa and the corresponding absorbance as the ordinate. b Determination
Weigh about 3g of the sample, accurate to 0.01g, transfer it to a 1000mL volumetric flask, add water to dilute to the mark, and shake the hook. Use a pipette to accurately transfer 50.00mL of the above solution, place it in a 250mL beaker, add water to 100mL, carefully add 2.0mL hydrogen peroxide (5.8.2.2c) and 2.0mL nitric acid solution (5.8.2.2a), and heat Evaporate until the volume of the solution is approximately 40 mL, cool to room temperature, completely transfer the solution to a 100 mL volumetric flask, add water to the mark, and shake well. Use the same working conditions as those used to measure the standard solution to measure its absorbance, and do a reagent blank test at the same time.
5.8.2. Expression of analysis results
The lead content (X,) expressed as a percentage of the amount is calculated according to formula (6): 2(m- no)
X 100| |tt||X,
m The absorbance of the reagent blank solution, the mass of lead detected from the working curve, m the mass of the sample·.
t5
5.8.2.6 Allowable difference
Take the arithmetic mean of the parallel measurement results as the measurement result. The absolute difference between the two parallel measurement results shall not be greater than 0.0003%. 6 Inspection Rules
6.1 Polyferric sulfate shall be inspected for product quality by the quality inspection department of the manufacturer in accordance with the test methods and inspection rules specified in this standard. The manufacturer shall ensure that all products shipped meet the requirements of this standard. . 6.2 Each batch of products leaving the factory should be accompanied by a quality instruction sheet, including: manufacturer name, product name, grade, batch number, production date, net 69
s
Hold: 5
Argon flow salt+ml./min
5.8.2.4 Analysis steps
200
20
10
300
FE
table?
ashing
600
1o
20
300
atomization
2300
1
5
50
Delete
2500
1
2
300
a, Drawing of working curve
Use pipettes to pipette 0.0, 1.0.3.0, 5.0.7.0, 9.0mL lead standard solutions (5.8.2.2e) respectively, place them in six 100mL volumetric flasks, and add nitric acid solution (5.8.2.2b) to the mark and spread evenly. According to the instrument manual, adjust the various conditions of the atomic absorption spectrometer to the optimal state. After zeroing with a reagent blank, measure the absorbance of each standard solution separately. Draw a working curve with the lead content as the abscissa and the corresponding absorbance as the ordinate. b Determination
Weigh about 3g of the sample, accurate to 0.01g, transfer it to a 1000mL volumetric flask, add water to dilute to the mark, and shake the hook. Use a pipette to accurately transfer 50.00mL of the above solution, place it in a 250mL beaker, add water to 100mL, carefully add 2.0mL hydrogen peroxide (5.8.2.2c) and 2.0mL nitric acid solution (5.8.2.2a), and heat Evaporate until the volume of the solution is approximately 40 mL, cool to room temperature, completely transfer the solution to a 100 mL volumetric flask, add water to the mark, and shake well. Use the same working conditions as those used to measure the standard solution to measure its absorbance, and do a reagent blank test at the same time.
5.8.2. Expression of analysis results
The lead content (X,) expressed as a percentage of the amount is calculated according to formula (6): 2(m- no)
X 100| |tt||X,
m The absorbance of the reagent blank solution, the mass of lead detected from the working curve, m the mass of the sample·.
t5
5.8.2.6 Allowable difference
Take the arithmetic mean of the parallel measurement results as the measurement result. The absolute difference between the two parallel measurement results shall not be greater than 0.0003%. 6 Inspection Rules
6.1 Polyferric sulfate should be inspected by the quality inspection department of the manufacturer in accordance with the test methods and inspection rules specified in this standard. The manufacturer should ensure that all products shipped meet the requirements of this standard. . 6.2 Each batch of products leaving the factory should be accompanied by a quality instruction sheet, including: manufacturer name, product name, grade, batch number, production date, net 69
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