HG/T 3696.2-2002 Preparation of impurity standard solutions for chemical separation of inorganic chemical products
Some standard content:
Record number: 10942-2002
HG/T3696.2-2002
This standard is formulated by adopting ISO6353-1:1982 "Chemical Analysis Reagents Part 1: General Analytical Methods". The main differences between this standard and ISO6353-1 are as follows: the number of impurity standard solutions has increased from 47 to 84. According to the actual situation of my country's inorganic chemical products, 37 impurity solutions such as palladium, platinum, tellurium, vanadium, zirconium, cadmium, lithium, saw, beryllium, gallium, gold, strontium, antimony, thallium, tungsten, selenium, tin, indium, germanium, ferrous iron, boron, carbon, silicon, chromate, acetate, carbon disulfide, silicon dioxide, carbon dioxide, hydrogen peroxide, phenol, methanol, acetone, furfural, glucose, salicylic acid, biuret, acetic anhydride, etc. have been added. There are some differences in the preparation methods, among which ammonium, arsenic, calcium, chromium, sodium, carbonate, chloride, hexafluorosilicate are different from those in ISO6353-1.
The standard solutions of impurities such as iron, magnesium, manganese, bismuth, mercury, nickel, potassium, cobalt, titanium, zinc, nitrogen, nitrate, and sulfate adopt the method of ISO6353-1, and also list another preparation method used in my country for many years. Bismuth, platinum, vanadium, chromium, arsenic, cobalt, aluminum, manganese, molybdenum, nickel, lead, copper, zinc, and iron are added with the method of using high-purity metal preparation. Appendix A of this standard is the appendix of the standard.
This standard was proposed by the Policy and Regulations Department of the former State Administration of Petroleum and Chemical Industry. This standard is under the technical jurisdiction of the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization. The drafting unit of this standard: Tianjin Chemical Research and Design Institute. The main drafters of this standard: Yao Jinjuan and Shi Jie. This standard is published for the first time.
This standard is entrusted to the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization for interpretation. 27
Chemical Industry Standard of the People's Republic of China
Inorganic chemical products
Preparations of standard solutions for chemical analysis1Scope
This standard specifies the preparation method of impurity standard solutions for chemical analysis of inorganic chemical products. HG/T3696.2—2002
This standard is applicable to the preparation of solutions containing accurate amounts of substances (elements, ions or molecules) in a volume, and is used for the determination of impurity content in inorganic chemical products. It can also be used for other chemical products. 2Cited standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T6682—1992 Specifications and test methods for water used in analytical laboratories (egvISO3696:1987) HG/T3696.1—2002 Preparation of standard titration solutions for chemical analysis of inorganic chemical products HG/T3696.3—2002 Preparation of preparations and products for chemical analysis of inorganic chemical products 3 General provisions
3.1 The water used in this standard shall comply with the third-grade water specified in GB/T6682 or above unless otherwise specified. 3.2 The purity of the reagents used in this standard shall be above analytical grade. Surface treatment shall be performed before use of easily oxidizable metals. 3.3 The standard solution for impurity determination shall be measured with a pipette, and the volume measured each time shall not be less than 1.00 mL. 3.4 The standard solution for impurity determination shall generally have a shelf life of twelve months at room temperature (15-25°C). When turbidity, precipitation or color change occurs, it shall be prepared anew.
3.5 The preparation methods of the impurity standard solutions specified in this standard are arranged in alphabetical order. 3.6 The volume of the stock solution prepared in the standard is for reference only. The user can adjust the preparation volume appropriately according to the amount used, but it must not be less than 100mL.
4 Preparation method
4.1 Unless otherwise specified, the impurity standard solution calculated based on metal elements (see Table 1) should be stored in an appropriate plastic bottle after preparation. Table 1 Impurity standard solution in terms of metal elements Name
Ammonium (NH4)
Preparation method
Weigh 1.483 g of ammonium chloride dried to constant weight at 105-110°C, drop it into water, transfer it into a 500 mL volumetric flask, dilute to the scale, shake the hook, Approved by the State Economic and Trade Commission of the People's Republic of China on September 28, 2002 Solution concentration
1 mL of solution contains 1 mg of ammonium (NH4)
Implementation on June 1, 2003
Palladium (Pd)
Ba
Bi
Platinum (Pe)
Te
Vanadium (V)
Calcium (Ca)
Zirconium (Zr)
Radium (Cd)
Chromium (Ct)
HG/T3696.2-2002
Table 1 (continued)
Preparation method
Weigh 0.833g of palladium chloride that has been dried at 105~110℃ for 1h, add 15mL of 1+4 hydrochloric acid solution to dissolve, transfer to a 500mL volumetric flask, dilute to the mark, and shake well. 1. Weigh 0.889g of strontium chloride (BaCl, ·2HO), dissolve it in water, transfer it to a 500mL volumetric flask, dilute to the mark, and shake well.
2. Weigh 0.718g of barium carbonate that has been dried to constant weight at 110℃ in advance, dissolve it in 1+4 hydrochloric acid solution, transfer it to a 500mL volumetric flask, dilute to the mark, and shake well. 1. Weigh 1.16g of bismuth nitrate [Bi(NO,)·5H20, dissolve it in 50mL of 1+4 nitric acid solution, transfer it to a 500mL volumetric flask, dilute to the mark, and shake well. 2. Weigh 0.100g of metallic bismuth, dissolve it in 6mL of nitric acid, boil it to remove nitrogen trioxide gas, transfer it to a 100mL volumetric flask, dilute to the mark, and add the solution. 1. Weigh 1.245g of potassium fluoroplatinate, dissolve it in water, transfer it to a 500mL volumetric flask, dilute to the mark, and shake well. wwW.bzxz.Net
2. Weigh 0.100g of high-purity metal, dissolve it in a small amount of aqua regia, evaporate it to near dryness on a water bath, add 5mL of salt, evaporate it to near dryness on a water bath, add 20mL of 1+1 hydrochloric acid to dissolve it, transfer it to a 100mL volumetric flask, dilute it to the mark, and shake it. Weigh 0.100g of metal vanadium, add 20~30mL of hydrochloric acid and a few drops of nitric acid, warm it to dissolve, transfer it to a 100mL volumetric flask, dilute it to the mark with 1+1 hydrochloric acid solution, and shake it well. 1. Weigh 1.150g of ammonium metavanadate, dissolve it in water (warm it if necessary), transfer it to a 500mL volumetric flask, dilute it to the mark, and spread it well. 2. Weigh 0.100g of metallic vanadium, dissolve it in nitric acid, transfer it to a 100mL volumetric flask, dilute it to the mark, and shake it well.
1. Weigh 1.249g of calcium carbonate dried to constant weight at 105-110℃, dissolve in 50mL of 1+3 hydrochloric acid solution, boil to remove carbon dioxide, cool, transfer to a 500mL volumetric flask, dilute to scale, and shake well.
2. Weigh 1.834g of calcium chloride (CaClz·2H:O), dissolve in water, transfer to a 500mL volumetric flask, dilute to scale, and shake well
Weigh 1.766g of zirconium oxychloride (ZrOClg·8H.O), add 150mL of 1+3 hydrochloric acid solution to dissolve, transfer to a 500mL volumetric flask, dilute to scale with 1+3 hydrochloric acid solution, and shake well. 1. Weigh 0.100g of high-purity cadmium metal, dissolve it in nitric acid, evaporate it to dryness on a water bath, add 5mL of 1+9 hydrochloric acid solution, evaporate it to dryness on a water bath, add 20mL of 1+9 hydrochloric acid to dissolve, transfer it to a 100mL volumetric flask, dilute it to the mark, and spread it evenly. 1. Weigh 1.867g of potassium chromate that has been dried at 105℃ for 1h, dissolve it in a small amount of water containing 1 drop of 100g/L sodium hydroxide solution, transfer it to a 500mL volumetric flask, dilute to the scale, and spread.
8. Weigh 1.414g of potassium dichromate that has been dried at 120℃ for 4h, dissolve it in water, transfer it to a 500mL volumetric flask, dilute to the scale, and shake well. 3. Weigh 0.100g high-purity chromium metal is dissolved in hydrochloric acid, transferred to a 100mL volumetric flask, diluted to the mark, and shaken.
Concentration of solution
1mL solution contains 1mg of palladium (Pd)
1mL solution contains 1mg of thorium (Ba)
1mL solution contains 1mg of (Bi)
1mL solution contains 1mg of platinum (Pt)
1mL solution contains 1mg of thorium (Te)
1mL solution contains 1mg of (V)
1mL solution contains 1mg of calcium (Ca)
1mL solution contains 1mg of zirconium (Ztr)
1mL solution contains 1mg of cadmium (Cd)
1mL L solution contains chromium (Cr) 1mg
mercury (Hg)
cobalt (Co)
ga (Ga)
potassium (K)
gold (Au)
lithium (Li)
aluminum (AI)
magnesium (Mg)
manganese (Mn)
HG/T3696.2—2002
Table 1 (continued)
Preparation method
1. Weigh 0.677g mercuric chloride, dissolve it in water, transfer it to a 500mL volumetric flask, dilute to the mark, and shake well.
2. Weigh 0.809g mercuric nitrate, dissolve it in 50mL of 1+9 nitric acid, transfer it to a 500mL volumetric flask, dilute to the mark, and shake well.
1. Weigh 1.315g of anhydrous cobalt sulfate (burned to constant weight at 500~550℃ with CoSO,7H,0), add 100mL of water, heat until dissolved, transfer to a 500mL volumetric flask after cooling, dilute to scale, and shake well.
2. Weigh 2.469g of cobalt nitrate [Co(NO),·6HO], dissolve in water, transfer to a 500mL volumetric flask, dilute to scale, and spread well. 3. Weigh 0.100g of high-purity cobalt metal, dissolve in nitric acid, evaporate to dryness on a water bath, add 5mL of 1+109 hydrochloric acid solution, evaporate to dryness on a water bath, add 20mL of 1+9 hydrochloric acid to dissolve, transfer to a 100mL volumetric flask, dilute to scale, and shake well. Weigh 0.665g of dichromate trioxide, dissolve in 25mL of sulfuric acid, transfer to a 500mL volumetric flask, carefully dilute to scale, and shake well.
1. Weigh 0.953g of potassium fluoride burned at 500-600℃ to constant weight, dissolve in water, transfer to a 500mL volumetric flask, dilute to scale, and spread evenly. 2. Weigh 1.293g of potassium nitrate, dissolve in water, transfer to a 500mL volumetric flask, dilute to scale, and shake evenly.
Weigh 0.100g of high-purity metal gold, add 10mL of hydrochloric acid and 5mL of nitric acid to dissolve, evaporate to near dryness on a water bath, dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, and shake to hook. Weigh 2.661g of lithium carbonate, add 50mL of water and 25mL of hydrochloric acid to dissolve, transfer to a 500mL volumetric flask, dilute to scale with water, and shake to hook. 1. Weigh 8.797g of potassium aluminum sulfate [AIK (SO.) 12H:O], dissolve it in water, add 50mL of 1+3 sulfuric acid solution, transfer it to a 500mL volumetric flask, dilute to the mark, and stir. 2. Weigh 0.100g of high-purity aluminum metal, dissolve it in hydrochloric acid, transfer it to a 100mL volumetric flask, dilute to the mark, and shake the spoon.
1. Weigh 0.829g of magnesium oxide burned to constant weight at 800℃, dissolve it in 10mL of hydrochloric acid and a small amount of water, transfer it to a 500mL volumetric flask, dilute to the mark, and shake well. 2. Weigh 5.070g of magnesium sulfate (MgSO·7H,0). Dissolve it in water, transfer it to a 500mL volumetric flask, dilute to the mark, and shake well.
1. Weigh 1.374g of anhydrous manganese sulfate burned to constant weight at 400~500℃, dissolve it in water, transfer it to a 500mL volumetric flask, dilute to scale, and shake well. 2. Weigh 1.538g of manganese sulfate (MnSO.·HO), dissolve it in water, transfer it to a 500mL volumetric flask, dilute to scale, and shake well.
3. Weigh 0.100g of high-purity manganese metal, dissolve it in 10mL of 1+1 nitric acid solution, evaporate it on a water bath until it is almost dry, add 5mL of 1+9 hydrochloric acid solution, evaporate it on a water bath until it is almost dry, add 20mL of 1+9 hydrochloric acid to dissolve it, transfer it to a 100mL volumetric flask, dilute to scale, and shake well. 1. Weigh 0.920g of ammonium molybdate [（NH,）Mo,Ou·4H,O], dissolve it in water, transfer it to a 500mL volumetric flask, dilute to scale, and shake well. 2. Weigh 0.100g of high-purity molybdenum metal, dissolve it in a small amount of aqua regia, evaporate it on a water bath until it is nearly dry, add 20mL of 1+1 hydrochloric acid solution to dissolve it, transfer it to a 100mL volumetric flask, dilute it to the scale with 1+1 hydrochloric acid solution, and spread it evenly.
Concentration of solution
1mL solution contains 1mg of Hg
1mL solution contains 1mg of Cobalt (Co)
1mL solution contains 1mg of Ga
1mL solution contains 1mg of Potassium (K)
1mL solution contains 1mg of Gold (Au)
1mL solution contains 1mg of Lithium (Li)
1mL solution contains 1mg of Aluminum (AI)
1mL solution contains 1mg of Magnesium (Mg)
1mL solution contains 1mg of Manganese (Mn)
1mL solution contains 1mg of Molybdenum (Mo)
Sodium (Na)
Nb
Nickel (Ni)
Be||Lead (Pb)
Arsenic (As)
Sr
Tallium (TI)
Titanium (Ti)
Sb
Iron (Fe)
HG/T3696.2--2002
Table 1 (continued)
Preparation method
Weigh 1.271 g of sodium fluoride burned at 500~600℃ to constant weight, dissolve it in water, transfer it into a 500mL volumetric flask, dilute to the scale, and shake well. Weigh 0.143g of mortar-ground saw pentoxide and 4g of powdered potassium pyrosulfate, place them in a quartz crucible, burn and melt at 600℃, take out and cool, heat and dissolve with 20mL of 150g/L tartaric acid solution. Transfer to a 100mL volumetric flask, dilute to scale and shake.
1. Weigh 3.365g of nickel ammonium sulfate [NiSO.·NH.), SO.·6H.OJ, dissolve in water, transfer to a 500mL volumetric flask, dilute to scale, and spread evenly. 2. Weigh 2.239g of nickel sulfate (NiSO·6H.O) or 2.393g of nickel sulfate (NiSO4·7H,O), dissolve in water, transfer to a 500mL volumetric flask, dilute to scale, and shake to hook. 3. Weigh 0.100g of high-purity nickel metal, dissolve it in a small amount of nitric acid, evaporate it on water until it is nearly dry, add 5ml of 1+1 hydrochloric acid solution, evaporate it on a water bath until it is nearly dry, add 20mL of 1+9 hydrochloric acid to dissolve it, transfer it to a 100mL volumetric flask, dilute it to the mark, and shake it evenly. Weigh 1.965g of beryllium sulfate (BeSO.·4H,O), dissolve it in water, add 1mL of sulfuric acid, transfer it to a 100mL volumetric flask, dilute it to the mark, and shake it evenly. 1. Weigh 0.799g of lead nitrate, add 50mL of 1+9 phosphoric acid solution to dissolve it, transfer it to a 500mL volumetric flask, dilute it to the mark, and shake it evenly. 2. Weigh 0.100g of high-purity lead metal, dissolve it in nitric acid, transfer it to a 100mL volumetric flask, dilute it to the mark, and shake it evenly.
Weigh 0.660g of strontium trioxide dried to constant weight in a sulfuric acid dryer, dissolve it in 6mL of 100g/L sodium hydroxide solution while warm, transfer it to a 500mL volumetric flask, dilute to the scale and rub it evenly.
Weigh 1.521g of strontium chloride (SrClz·6H.O), dissolve it in water, transfer it to a 500mL volumetric flask, dilute to the scale and shake it evenly.
Weigh 0.587g of cerium chloride, dissolve it in 25mL of sulfuric acid, transfer it to a 500mL volumetric flask, dilute to the scale and shake it evenly.
1. Weigh 0.834g titanium dioxide, add 5~8g potassium pyrosulfate, burn and melt at 600℃, cool, dissolve with (1+35 sulfuric acid solution, transfer to 500mL volumetric flask, dilute to scale, shake well.
2. Weigh 2.147g titanium trioxide solution 150g/L, add 20mL 2+1 hydrochloric acid solution, transfer to 100mL volumetric flask, dilute to scale, shake well. Weigh 1.371g potassium antimony tartrate (C,HKO.Sb ·1/2H,O), dissolve in 1+3 hydrochloric acid solution, transfer to a 500mL volumetric flask, dilute to scale with 1+3 hydrochloric acid solution, and mix well. 1. Weigh 0.100g high-purity metallic iron (99.5% or more), add 15mL hydrochloric acid to dissolve, add 35 drops of 3% hydrogen peroxide, heat, and evaporate the solution to a volume of about 10mL. After cooling, transfer to a 100mL volumetric flask, dilute to scale, and mix well. 2. Weigh 4.317g ammonium ferric sulfate [NHFe (SO.）z, 12HO], dissolved in water, add 25mL of 1+6 sulfuric acid solution, transfer to a 500mL volumetric flask, dilute to scale, and spread evenly. Solution concentration
1mL solution contains sodium (Na) 1mg
1mL solution contains saw (Nb) 1mg
1mL solution contains nickel (Ni) 1mg
1mL solution contains benzene (Be) 1mg mg
1mL solution contains 1mg of lead (Pb)
1mL solution contains 1mg of arsenic (As)
1mL solution contains 1mg of strontium (Sr)
1mL solution contains 1mg of titanium (TI)
1mL solution contains 1mg of titanium (Ti)
1mL solution contains 1mg of antimony (Sb)
1mL solution contains 1mg of iron (Fe)
copper (Cu)
tungsten (W))||tt| |Selenium (Se)
Tin (Sn)
Zinc (Zn)
Iron II (Fe)
Indium (In)
Silver (Ag)
Germanium (Ge)
HG/T3696.2--2002
Table 1 (end)
Preparation method
1. Weigh 1.965g copper sulfate (CuSO5HzO), dissolve it in water, transfer it into a 500mL volumetric flask, dilute to the mark, and shake it.
2. Weigh 0.100g high-purity copper metal, dissolve it in nitric acid, evaporate it to dryness on a water bath, add 5mL hydrochloric acid, evaporate it to dryness on a water bath, add 20mL 1+9 hydrochloric acid to dissolve it, transfer it into a 100mL volumetric flask, dilute it to the mark, and shake it. Weigh 0.631g of tungsten trioxide that has been dried at 105~110℃ for 1h, add 3040mL of 200g/L sodium hydroxide, heat to dissolve, cool, transfer to a 500mL volumetric flask, dilute to scale, and shake well.
Note: It can be prepared by using ammonium tungstate that is burned at 400~500℃ for 20min and then decomposed to generate tungsten trioxide.
Weigh 0.703g of selenium dioxide, dissolve it in water, transfer it to a 500mL volumetric flask, dilute to scale, and shake well.
Weigh 0.100g of metallic tin, dissolve it in 1+1 hydrochloric acid solution, transfer it to a 100mL volumetric flask, dilute to scale with 1+1 hydrochloric acid solution, and shake well. 1. Weigh 0.622g of zinc oxide, dissolve it in 10mL of water and 5mL of sulfuric acid, transfer it to a 500mL volumetric flask, dilute to scale, and shake well. 2. Weigh 2.199g zinc sulfate (ZnSO·7H.O), dissolve it in water, transfer it to a 500mL volumetric flask, dilute to the mark, and shake well.
3. Weigh 0.100g high-purity zinc metal, dissolve it in hydrochloric acid, transfer it to a 100mL volumetric flask, dilute to the mark, and spread it well.
Weigh 0.702g ferrous ammonium sulfate [(NH), Fe(SO)2·6H,OJ, dissolve it in water containing 1mL of 1+1 sulfuric acid, transfer it to a 100mL volumetric flask, dilute to the mark, and shake well. This standard solution is prepared before use.
Weigh 0.100g high-purity steel metal, add 15mL of 1+1 hydrochloric acid solution, heat to dissolve, cool, transfer it to a 100mL volumetric flask, dilute to the mark, and shake well. Weigh 0.157g silver nitrate, dissolve it in water, transfer it to a 100mL volumetric flask, dilute to scale, and shake well. Store in a brown bottle.
Weigh 0.100g high-purity metal zirconium, heat and dissolve it in 3~5mL of 30% hydrogen peroxide, add nitrogen water drop by drop until the white precipitate dissolves, neutralize it with 1+4 sulfuric acid solution and add 0.5mL in excess, transfer it to a 100mL volumetric flask, dilute to scale, and shake well. 4.2 Standard solution of impurities based on non-metallic elements Unless otherwise specified, this impurity standard solution (see Table 2) should be stored in a glass bottle after preparation. Table 2 Standard solution of impurities based on non-metallic elements weighs
Nitrogen (N)
Preparation method
1. Weigh 0.382g ammonium fluoride dried to constant weight at 100~105℃, dissolve it in water, transfer it to a 100ml volumetric flask, dilute to scale, and shake well. 2. Weigh 0.607g sodium nitrate, dissolve it in water, transfer it to a 100mL volumetric flask, dilute to the mark, and shake well.
Concentration of solution
1mL solution contains 1mg copper (Cu)
1mL solution contains 1mg tungsten (W)
1mL solution contains 1mg selenium (Se)
1mL solution contains 1mg Sn
1mL solution contains 1mg zinc (Zn)
1mL solution contains 1mg ferrous iron (Fe)
1mL solution contains 1mg indium (In)
1mL solution contains 1mg silver (Ag)
1mL solution contains 1mg silver (Ag) Solution contains 1mg of galvanic acid (Ge)
Concentration of solution
1mL solution contains 1mg of oxygen (N)
Silicon (Si)
Phosphorus (P)
Sulfur (S)
(CI))
Boron (B)
Carbon (C)
HG/T3696.2—2002
Table 2 (end)
Preparation method
Weigh 0.214g of silicon dioxide, place it in platinum, add 1g of anhydrous sodium carbonate, and mix well. Heat at 1000℃ until completely melted, cool, dissolve in water, transfer to a 100mL volumetric flask, dilute to the mark, and shake well. Store in a polyethylene bottle Weigh 0.439g of potassium dihydrogen phosphate, dissolve in water, transfer to a 100mL volumetric flask, dilute to the mark, and shake well.
Weigh 0.544g potassium sulfate, dissolve it in water, transfer it to a 100mL volumetric flask, dilute to the mark, and spread it evenly.
Weigh 3.97g nitrogen amine T (C,H,CINNeO,S.3HO), place it in a 100mL volumetric flask, dissolve it in water, dilute to the mark, and shake it evenly. Weigh 0.572g boric acid, add 50mL water, dissolve it in warm water, transfer it to a 100mL volumetric flask, dilute to the mark, and shake it evenly.
Weigh 0.883g anhydrous sodium carbonate burned to constant weight at 270~300℃, dissolve it in water without carbon dioxide, transfer it to a 100mL volumetric flask, dilute to the mark with water without carbon dioxide, and shake it evenly.
4.3 Impurity standard solution based on acid ions
Unless otherwise specified, this impurity standard solution (see Table 3) should be stored in a glass bottle after preparation. Table 3 Impurity standard solution based on acid radical ions
Oxalate
Iodide
Iodate
Fluoride
Chromate
Silicate
Phosphate
Thiosulfate
Sulfide
Preparation method
Weigh 0.143g oxalic acid (CH,O·2HO), dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, shake well
Weigh 0.131g potassium iodide, dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, shake well. Store in a brown bottle.
Weigh 0.122g potassium iodate, dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, shake well. Store in a brown bottle.
Weigh 0.221g sodium fluoride, dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, and shake well. Store in a polyethylene bottle.
Weigh 0.167g potassium chromate dried at 105~110℃ for 1h, dissolve in a small amount of water containing 1 drop of 100g/L sodium hydroxide solution, transfer to a 100mL volumetric flask, dilute to scale, and shake well.
Weigh 0.790g silicon dioxide, place in a platinum crucible, add 2.6g anhydrous sodium carbonate, and mix well. Heat at 1000℃ until completely melted, cool, dissolve in water, transfer to a 1000mL volumetric flask, dilute to scale, and shake well. Store in a polyethylene bottle. Weigh 0.143g potassium dioxygen phosphate, dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, and shake well.
Weigh 0.221g sodium thiosulfate (NaSO, 5H2O). Dissolve in boiled water, transfer to a 100mL volumetric flask, dilute to scale with boiled water, and shake well. Weigh 0.749g sodium sulfide (Na2S.9HO), dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, and shake well. This standard solution is prepared before use. Solution concentration
1mL solution contains 1mg silicon (Si)
1mL solution contains 1mg phosphorus (P)
1mL solution contains 1mg sulfur (S)
1mL solution contains 1mg chlorine (CI)
1 mL solution contains 1mg boron (B)
1mL solution contains 1mg carbon (C)
Solution concentration
1mL solution contains 1mgCz0.
1 mL.The solution contains 1 mgI
1 mL of solution contains 1 mg10
1 mL of solution contains 1 mgF
1 mL of solution contains 1 mgCrO4
1 mL of solution contains 1 mgSiO
1 mL of solution contains 1 mgPO
1 mL of solution contains 1 mgS.0
1 mL of solution contains 1 mg S
Thiocyanate
Sulfate
Hexafluorosilicate
Hexacyanoferrate
(II) acid salt
Chloride
Chlorate
Carbonate
Nitrate
Bromide
Bromoate
Nitrite
HG/T3696.2—2002
Table 3 (end)
Preparation method
Weigh 0.131g of ammonium thiocyanate, dissolve it in water, transfer it to a 100mL volumetric flask, dilute to the mark, and shake well.
1. Weigh 0.148g of anhydrous sodium sulfate dried to constant weight at 105~110℃, dissolve it in water, transfer it to a 100mL volumetric flask, dilute to the mark, and mix well. 2 Weigh 0.181g potassium sulfate, dissolve it in water, transfer it to a 100mL volumetric flask, dilute to the mark, and shake well.
Weigh 30%~32% hexafluorosilicic acid mg, dissolve it in water, transfer it to a 100mL volumetric flask, dilute to the mark, and shake well. This standard solution is stored in a polyethylene bottle. The mass of hexafluorosilicic acid is calculated according to the following formula:
1.0141X0.1000
Where: Milk - the mass of hexafluorosilicic acid, g; X - the actual percentage of hexafluorosilicic acid; 0.1000 - the mass of hexafluorosilicic acid required to prepare 100mL of hexafluorosilicic acid impurity standard solution, g.
Note: Before preparation, the content of hexafluorosilicic acid should be determined according to the method specified in A2 of Appendix A of this standard.
Weigh 0.199g potassium hexacyanoferrate (K.[Fe(CN)·3H2O), dissolve in water. Transfer to a 100mL volumetric flask, dilute to scale, and spread evenly. Weigh 0.165g sodium chloride burned to constant weight at 500-600℃, dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, and shake well. Weigh 0.147g potassium chloride, dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, and shake well.
Weigh 0.177g anhydrous sodium carbonate burned to constant weight at 270-300℃, dissolve in water without carbon dioxide, transfer to a 100mL volumetric flask, dilute to scale with water without carbon dioxide, and shake well.
1. Weigh 0.163g potassium nitrate dried to constant weight at 120~130℃, dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, and shake well. 2. Weigh 0.137g sodium nitrate, dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, and shake well.
Weigh 0.149g potassium bromide, dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, and shake well. Store in a brown bottle.
Weigh 0.131g potassium bromate, dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, and shake well. Store in a brown bottle.
Weigh 0.150g sodium nitrite, dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, and shake well. This solution is prepared before use. Weigh 2.305g sodium acetate (CHCOON&·3H:O), dissolve it in water, transfer it into a 100mL volumetric flask, dilute to the mark, and shake well. 4.4 Standard solution of impurities by molecule
Unless otherwise specified, this standard solution of impurities (see Table 4) should be stored in a glass bottle after preparation. Solution concentration
1 mL of solution contains 1mgSCN
1 mL of solution contains 1mgSO
1 mL of solution contains 1mgSiF.
1mL of solution contains 1mgFeCN).
1mL solution contains 1mgCI
1mL solution contains 1mgCIO
1mL solution contains 1mgCO
1mL solution contains 1mgNO.
1mL solution contains 1 mg Br
1mL solution contains 1mgBrO
1mL solution contains 1 mgNOz
1mL solution contains 1mgCH,CO0O
Carbon disulfide
Silicon dioxide
Carbon dioxide
Hydrogen peroxide
Glucose
HG/T3696.2—2002
Table 4 Impurity standard solution in terms of molecules
Preparation method
Weigh 0.100g acetone, dissolve it in water, transfer it into a 100mL volumetric flask, dilute to the mark, and spread evenly. This standard solution is prepared before use. Weigh 0.500g of carbon disulfide, dissolve it in carbon tetrachloride, transfer it to a 500mL volumetric flask, dilute it to the mark with carbon tetrachloride, and shake it. This standard solution is prepared before use. 1. Weigh 0.100g of silicon dioxide, place it in platinum, add 1g of anhydrous sodium carbonate, and shake it. Heat it at 1000℃ until it is completely melted, cool it, dissolve it in water, transfer it to a 100mL volumetric flask, dilute it to the mark, and shake it well. Store it in a polyethylene bottle. 2. Weigh 0.100g of silicic acid that has been burned to constant weight at 900℃ in advance, dissolve it in 8mL of 30g/L sodium hydroxide solution, transfer it to a 100mL volumetric flask, dilute it to the mark, and shake it well. Store it in a polyethylene bottle.
Weigh 0.240g of anhydrous sodium carbonate burned to constant weight at 270~300℃, dissolve in water with no solution concentration
1mL solution contains 1mgCH.COCHa
1mL solution contains 1mg CSs
1mL solution contains 1mgSiOz
1mL solution contains 1mgCO, or 0.27
carbon dioxide, transfer to a 100mL volumetric flask, dilute mgc
to the mark with water without carbon dioxide, and shake well.
Weigh 0.100g of benzene, dissolve in water, transfer to a 100mL volumetric flask, dilute to the mark, and shake well.
Weigh mg of 30% hydrogen peroxide, place in a 100mL volumetric flask, dilute to the mark, and shake well. This standard solution is prepared before use. The mass of 30% hydrogen peroxide is calculated as follows;
wherein·m
The mass of 30% hydrogen peroxide, g:
-The actual percentage of 30% hydrogen peroxide; The mass of hydrogen peroxide required to prepare 100mL of hydrogen peroxide impurity standard solution, g.
Note: Before preparation, the content of 30% hydrogen peroxide should be determined according to the method specified in A3 of Appendix A of this standard.
Weigh 0.100 methanol, dissolve it in water, transfer it into a 100mL volumetric flask, dilute to the scale, and shake it evenly. This standard solution is prepared before use. Weigh mg formaldehyde solution, place it in a 100mL volumetric flask, dilute to the scale, and shake it evenly. This standard solution is prepared before use.
The mass of formaldehyde solution is calculated as follows:
Where: m
The mass of formaldehyde solution, g;
The actual percentage of dissolved formaldehyde
-The mass of formaldehyde required to prepare 100ml. Formaldehyde impurity standard solution·g.
Note: Before preparation, the formaldehyde content should be determined according to the method specified in A4 in Appendix A of this standard.
Weigh 0.100g of aldehyde, dissolve it in water, transfer it to a 100mL volumetric flask, dilute it to the mark, and shake it well.
Weigh 0.100g of glucose, dissolve it in water, transfer it to a 100mL volumetric flask, dilute it to the mark, and shake it well.
1mL solution contains 1mgCHOH
1mL solution contains 1mgH,0
1ml. solution contains 1mgCH,OH
1mL solution contains 1mgHCHO
1mL solution contains 1mgC,H.0
1ml. solution contains 1mgCHQ·H,0
Salicylic acid
Diptera polysaccharide||t t||Thenyl compounds
Acetic anhydride
HG/T3696.2--2002
Table 4 (end)
Preparation method
Weigh 0.100g salicylic acid, add a small amount of water and 1mL glacial acetic acid, transfer to a 100mL volumetric flask, dilute to scale, and mix well. Weigh 0.100g dihydrogen sulfoxide, dissolve in water, transfer to a 100mL volumetric flask, dilute to scale, and shake well. This standard solution is prepared before use. Weigh 10.43g acetone (equivalent to 5,000gCO) and place in a 100mL volumetric flask containing 50mL carbonyl-free methanol, dilute to scale with carbonyl-free methanol, and shake well. Transfer 2.00mL of this solution is placed in a 100mL volumetric flask, diluted to the mark with carbonyl-free methanol, and the standard solution is prepared before use. Weigh 40% acetaldehyde solution mg, place it in a 100mL volumetric flask, dilute to the mark, and the standard solution is prepared before use. The mass of 40% acetaldehyde is calculated as follows:
Where: m——the mass of 40% acetaldehyde·g; X——the actual percentage of 40% acetaldehyde; 0.1000——the mass of acetaldehyde required to prepare 100mL acetaldehyde impurity standard solution, g.
Note: Before preparation, the content of 40% acetaldehyde should be determined according to the method specified in A1 in Appendix A of this standard.
Weigh 0.100g of acetic anhydride, dissolve it with glacial acetic acid without acetic anhydride, transfer it to a 100mL volumetric flask, dilute to the mark with glacial acetic acid without acetic anhydride, and shake well. This standard solution is prepared before use.
Note: Preparation of glacial acetic acid without acetic anhydride. Reflux glacial acetic acid for half an hour and distill to obtain
Concentration of solution
1mL solution contains 1mgHOCH,COOH
1mL solution contains 1mgNH,CONHCONH
1mL solution contains 1mgCO
1mL solution contains 1mgCH,CHO
1mL solution contains 1mg(CH,CO)20
A140% acetaldehyde solution content determination
HG/T3 696.2--2002
Appendix A
(Appendix of the standard)
Methods for determination of the contents of four solutions
Measure 50.00mL of hydroxylamine fluoride solution [c (NH.OH·HCI=2mol/L)] and inject it into a stoppered conical flask, weigh it, add 1.5mL of acetaldehyde, let it stand for 30min, weigh it again, and weigh it twice with an accuracy of 0.0002g. Add 10 drops of bromophenol blue indicator solution, and titrate it with sodium hydroxide standard titration solution [c (NaOH)=1mol/L], and do a blank test at the same time. The blank test is to measure 50.00mL of hydroxylamine fluoride solution Lc (NHzOH·HCI=2mol/L)], add 30mL of water, and perform the same operation as the sample.
40% acetaldehyde content is calculated according to formula (A1):
X;=(Vi-V.)cX0. 044 05
Wherein: X
40% acetaldehyde solution percentage, %; the amount of sodium hydroxide standard titration solution, mL-blank test the amount of sodium hydroxide standard titration solution, mL: the actual concentration of sodium hydroxide standard titration solution, mol/L; (A1)
40% acetaldehyde mass, g;
and 1.00mL sodium hydroxide standard titration solution [c(NaOH=1.000mol/L)] The mass of acetaldehyde expressed in grams.
A2 Hexafluorosilicic acid content determination
Weigh 3g hexafluorosilicic acid (accurate to 0.0002g). Place in a polyethylene cup, add 100mL of water, 10mL of saturated potassium chloride solution and 3 drops of 10g/L phenol indicator solution, cool to 0℃, titrate with sodium hydroxide standard solution [e(NaOH)=1mol/L] until pink, keep for 15s(V,). Then heat to 80℃, continue to titrate with sodium hydroxide standard titration solution [c(NaOH)=1mol/L] until the solution turns stable pink (V,).
The content of hexafluorosilicic acid is calculated according to formula (A2): XxYac×0.03602×100
（A2)
Wherein, X is the percentage of hexafluorosilicic acid, %; V. —The amount of sodium hydroxide standard titration solution titrated to the second endpoint, mL; the actual concentration of sodium hydroxide standard titration solution, mol/L; the mass of hexafluorosilicic acid, g;
0.03602—The mass of hexafluorosilicic acid expressed in grams equivalent to 1.00mL sodium hydroxide standard titration solution [c(NaOH)=1.000mol/L.
A330% Hydrogen Peroxide Content Determination
Measure 1.8mL (2g) of 30% hydrogen peroxide, inject it into a stoppered conical flask (accurate to 0.0002g), transfer it to a 250mL volumetric flask, dilute to the scale, and spread it evenly. Measure 25.00mL of it, add 10mL of 20% sulfuric acid solution, and titrate with potassium permanganate standard titration solution [c(1/5KMnO.)] until the solution turns pink, and keep it for 30s. The content of 30% hydrogen peroxide is calculated according to formula (A3): 38
HG/T3696.2—2002
X,=Vc×0.017.01×100
Wherein: X—the percentage of 30% hydrogen peroxide, %; V——the amount of standard potassium permanganate titration solution, mL; C—the actual concentration of standard potassium permanganate titration solution, mol/L; m—the mass of 30% hydrogen peroxide, g
(A3)
—the mass of hydrogen peroxide expressed in grams equivalent to 1.00mL standard potassium permanganate titration solution Lc (KMnO,) = 1.000mol/L.
A4 Determination of formaldehyde solution content
Measure 3mL of formaldehyde solution (accurate to 0.0002g), add it to 50mL of sodium sulfite solution [c(NaaSO.)=1mol/L, and titrate it with sulfuric acid standard titration solution [c(1/2H2SO.)] until the solution changes from blue to colorless. The formaldehyde solution content is calculated according to formula (A4):
X,=YcX0. 030 03x100
Where: X—the percentage of formaldehyde solution, %; V-
the amount of sulfuric acid standard titration solution, mL; c the actual concentration of sulfuric acid standard titration solution, mol/L; - the mass of formaldehyde solution, g;
the mass of formaldehyde in grams equivalent to 1.00mL of sulfuric acid standard titration solution [c(1/2HzSO)=1.000mol/L).
Note: Preparation of sodium sulfite solution [c(NazSO, = 1 mol/L)]: weigh 126g sodium sulfite, dissolve in water, dilute to 1000mL, add 1mol/L thymol indicator solution, and neutralize with 1+30 sulfuric acid solution until colorless.000mol/L)] is equivalent to the mass of acetaldehyde expressed in grams.
A2 Determination of hexafluorosilicic acid content
Weigh 3g of hexafluorosilicic acid (accurate to 0.0002g). Place in a polyethylene cup, add 100mL of water, 10mL of saturated potassium chloride solution and 3 drops of 10g/L phenol indicator solution, cool to 0℃, and titrate with sodium hydroxide standard solution [e(NaOH)=1mol/L] until it turns pink, and keep for 15s (V,). Then heat to 80℃, and continue to titrate with sodium hydroxide standard titration solution [c(NaOH)=1mol/L] until the solution turns a stable pink (V,).
The content of hexafluorosilicic acid is calculated according to formula (A2): XxYac×0.03602×100
（A2)
Wherein, X——the percentage of hexafluorosilicic acid, %; V. —The amount of sodium hydroxide standard titration solution titrated to the second endpoint, mL; the actual concentration of sodium hydroxide standard titration solution, mol/L; the mass of hexafluorosilicic acid, g;
0.03602—The mass of hexafluorosilicic acid expressed in grams equivalent to 1.00mL sodium hydroxide standard titration solution [c(NaOH)=1.000mol/L.
A330% Hydrogen Peroxide Content Determination
Measure 1.8mL (2g) of 30% hydrogen peroxide, inject it into a stoppered conical flask (accurate to 0.0002g), transfer it to a 250mL volumetric flask, dilute to the scale, and spread it evenly. Measure 25.00mL of it, add 10mL of 20% sulfuric acid solution, and titrate with potassium permanganate standard titration solution [c(1/5KMnO.)] until the solution turns pink, and keep it for 30s. The content of 30% hydrogen peroxide is calculated according to formula (A3): 38
HG/T3696.2—2002
X,=Vc×0.017.01×100
Wherein: X—the percentage of 30% hydrogen peroxide, %; V——the amount of standard potassium permanganate titration solution, mL; C—the actual concentration of standard potassium permanganate titration solution, mol/L; m—the mass of 30% hydrogen peroxide, g
(A3)
—the mass of hydrogen peroxide expressed in grams equivalent to 1.00mL standard potassium permanganate titration solution Lc (KMnO,) = 1.000mol/L.
A4 Determination of formaldehyde solution content
Measure 3mL of formaldehyde solution (accurate to 0.0002g), add it to 50mL of sodium sulfite solution [c(NaaSO.)=1mol/L, and titrate it with sulfuric acid standard titration solution [c(1/2H2SO.)] until the solution changes from blue to colorless. The formaldehyde solution content is calculated according to formula (A4):
X,=YcX0. 030 03x100
Where: X—the percentage of formaldehyde solution, %; V-
the amount of sulfuric acid standard titration solution, mL; c the actual concentration of sulfuric acid standard titration solution, mol/L; - the mass of formaldehyde solution, g;
the mass of formaldehyde in grams equivalent to 1.00mL sulfuric acid standard titration solution [c(1/2HzSO)=1.000mol/L).
Note: Preparation of sodium sulfite solution [c(NazSO, = 1 mol/L)]: weigh 126g sodium sulfite, dissolve in water, dilute to 1000mL, add 1mol/L thymol indicator solution, and neutralize with 1+30 sulfuric acid solution until colorless.000mol/L)] is equivalent to the mass of acetaldehyde expressed in grams.
A2 Determination of hexafluorosilicic acid content
Weigh 3g of hexafluorosilicic acid (accurate to 0.0002g). Place in a polyethylene cup, add 100mL of water, 10mL of saturated potassium chloride solution and 3 drops of 10g/L phenol indicator solution, cool to 0℃, and titrate with sodium hydroxide standard solution [e(NaOH)=1mol/L] until it turns pink, and keep for 15s (V,). Then heat to 80℃, and continue to titrate with sodium hydroxide standard titration solution [c(NaOH)=1mol/L] until the solution turns a stable pink (V,).
The content of hexafluorosilicic acid is calculated according to formula (A2): XxYac×0.03602×100
（A2)
Wherein, X——the percentage of hexafluorosilicic acid, %; V. —The amount of sodium hydroxide standard titration solution titrated to the second endpoint, mL; the actual concentration of sodium hydroxide standard titration solution, mol/L; the mass of hexafluorosilicic acid, g;
0.03602—The mass of hexafluorosilicic acid expressed in grams equivalent to 1.00mL sodium hydroxide standard titration solution [c(NaOH)=1.000mol/L.
A330% Hydrogen Peroxide Content Determination
Measure 1.8mL (2g) of 30% hydrogen peroxide, inject it into a stoppered conical flask (accurate to 0.0002g), transfer it to a 250mL volumetric flask, dilute to the scale, and spread it evenly. Measure 25.00mL of it, add 10mL of 20% sulfuric acid solution, and titrate with potassium permanganate standard titration solution [c(1/5KMnO.)] until the solution turns pink, and keep it for 30s. The content of 30% hydrogen peroxide is calculated according to formula (A3): 38
HG/T3696.2—2002
X,=Vc×0.017.01×100
Wherein: X—the percentage of 30% hydrogen peroxide, %; V——the amount of standard potassium permanganate titration solution, mL; C—the actual concentration of standard potassium permanganate titration solution, mol/L; m—the mass of 30% hydrogen peroxide, g
(A3)
—the mass of hydrogen peroxide expressed in grams equivalent to 1.00mL standard potassium permanganate titration solution Lc (KMnO,) = 1.000mol/L.
A4 Determination of formaldehyde solution content
Measure 3mL of formaldehyde solution (accurate to 0.0002g), add it to 50mL of sodium sulfite solution [c(NaaSO.)=1mol/L, and titrate it with sulfuric acid standard titration solution [c(1/2H2SO.)] until the solution changes from blue to colorless. The formaldehyde solution content is calculated according to formula (A4):
X,=YcX0. 030 03x100
Where: X—the percentage of formaldehyde solution, %; V-
the amount of sulfuric acid standard titration solution, mL; c the actual concentration of sulfuric acid standard titration solution, mol/L; - the mass of formaldehyde solution, g;
the mass of formaldehyde in grams equivalent to 1.00mL of sulfuric acid standard titration solution [c(1/2HzSO)=1.000mol/L).
Note: Preparation of sodium sulfite solution [c(NazSO, = 1 mol/L)]: weigh 126g sodium sulfite, dissolve in water, dilute to 1000mL, add 1mol/L thymol indicator solution, and neutralize with 1+30 sulfuric acid solution until colorless.
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