Some standard content:
1CS71.100
Classification number: G71
Reserve number: 12501-2003
Light Industry Standard of the People's Republic of China
QB/T1768—2003
Replaces QB/T176R—1993
4A Zeolite for Detergents
4A Zcolite for detergents
Issued on September 13, 2003
National Development and Reform Commission of the People's Republic of China Implemented on October 1, 2003
This standard is a revision of QB/1768-1993 4A Zeolite for Detergents. The main changes of this standard QR/T1768-199 are as follows: the physical and chemical performance classification is cancelled; the test method for calcium transfer ability is specified; the test method for loss on burning is added; the average efficiency index is added; the density index is added; the resting treatment index is added; the AI ≥ 10 index is added; this standard is attached A and D. This standard is proposed by the China Light Industry Federation. This standard is under the jurisdiction of the National Center for Standardization of Surface Treatment Cleaning Products. QB/T1768—2J03
This standard is mainly drafted by: Ningxia Chemical Industry Co., Ltd. Shandong Branch Aluminum Chemical Co., Ltd. National Institute of Daily Chemical Industry. The main drafter of this international standard is Zhao Bing, who was first revised and issued in 1933. This is the first revision. This international standard will be implemented from 1993. QB/T1768-1993 4A zeolite for detergents
1 Scope
4A zeolite for detergents
Q/T*768-2003
This standard specifies the requirements, test methods, inspection plan, marking, packaging, transportation and storage of 4A zeolite for detergents. This standard certifies the use of 4A zeolite for detergents and 4A zeolite for other purposes. 2 Normative references The following documents are used as international standards through unmarked reference. If the date of the reference is not specified, all subsequent amendments (excluding errors) or revisions to the referenced document are not valid for use in this standard. However, the parties who have reached an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For any unmarked referenced document, the latest version shall apply. GB601:2002 Standard for the preparation of titration solutions of chemical reagents GB636, Determination of pH value of aqueous surfactants. Support method GB/T11986 Determination of the angle of repose of surfactant powder and particle wall GB/T13175 Determination of the effect of detergent on the performance of the powder GB/T 13176.1
Determination of the effect of detergent on the performance of the powder
3 Terms and definitions
Many technical specifications and definitions apply to this standard.
Ignition loss
44 Boiling point The percentage of particles that decrease when burned at high temperatures. 3.2
Half mean diameter
The average diameter of a particle group composed of 4A and 4A particles. $. 3
Particle distribution The percentage of particles with the same particle size in the total particle size. 3.4
Density
In the standard object, the unit volume of the bamboo is required or the micro-quality is required, expressed as m. 4 Requirements
4.1 Appearance
It should be colorless, odorless, and free of foreign matter and light. 4.2: Chemical composition
Detergent 4A is a type of sodium aluminate, the chemical composition is: Na% L (A1 (ys (Si02)%) · 216H04.3 Type
Type 4A is a type of sodium aluminate that can be connected to the environment. Its quantitative identification technology is QB/T1768-2003
Physical and chemical properties
Detergent 4A should comply with the physical and chemical properties of the standard. Table 1 Physical and chemical properties of detergent 4A zeolite
Calcium crosslinking energy C/,
P average detection, m
PH 1X. 25T.J
RIP, 1h, %
Relaxation, yr
Resting time, (\)
Testing method
Unless otherwise specified, only water with a purity higher than that of the analytical reagent and distilled water or water with a purity higher than that of water shall be used in the analysis. 5.1 Determination of loss on ignition
5.1.1 Principle
4A is not used under high humidity at 800℃. According to the change of quality before and after the furnace, the burning head is calculated. 5.1.2 Apparatus
High temperature protection, automatic temperature control (80010)T: a
Reagent ratio, 30mL;
Drying machine, filled with antibacterial desiccant.
5. 1. 3 Weighing the sample
Weigh the sample 1 (length 0.1mg) and put it into the porcelain tube (5.1.26) 1, and use two to measure the burning zone in parallel. 5.1.4 Determination
Place the weighed sample in a high-temperature furnace, and start timing when the temperature rises to ±1 °C. Burn for 1 hour, turn off the power and place the sample in a dry device to cool to the actual temperature, weigh it, and make sure the temperature reaches 0.1m. The average fire environment is expressed as a percentage, and the connection method is (x(%) = mm ×100
Formula +,
average sample quality before calcination, g!
sample quality after calcination, E.
to calculate the average value of the clothes to the number of digits ()
anti-density: the single set of complex recordings must be obtained under the conditions of the independent test results to protect the difference of 0.5%, the situation of 0.5% does not exceed 5% as a prerequisite.
5.2 Determination of calcium conversion capacity
child B specification determination
5.3 Determination of resolution
determined according to the provisions of double C
5.4 Determination of whiteness
according to GB /T13176.1 standard determination.
The result is expressed as the technical mean value to one decimal place. QB/T1769·2C93
Density: The difference between the two independent tests obtained in the test piece is not allowed to exceed 0.5%, with a 0.5% error.
5.5PH determination
according to GB/T6368, the accuracy is 0.U2pH. 1.0 (accurate 0.1), 100ml of sample, add 100m water, stir and keep stirring, keep stirring at 25℃ for 6 seconds, and keep stirring at the same time. The result is expressed as the technical mean value to one decimal place. Solution: The difference between the values of the warranties issued under the annualized conditions shall not be less than 6.111 units, provided that the value of the warranties does not exceed 5 units under the condition of 0.pH.
5.6 Determination of AI
Determination shall be made in accordance with the provisions of Insurance D.
5.7 Determination of bulk density
Determination shall be made in accordance with the provisions of GB/T13175, and the results shall be expressed in integers of the decimal places. Abstract rate: under the repeated occurrence conditions, the difference of the test results within the same test shall not exceed 50mg/mL, with the maximum value being 50mg/mT, and the condition where the difference does not exceed 5%.
5.% rest determination
Determine according to the provisions of GB[1986], convert the test result to 1B and calculate the average result at the end, round to the integer: Other rates: under the repeated occurrence conditions, the difference of the test results within the same test shall not exceed 1.3°, with the condition where the difference does not exceed 1.3% as the initial value:
6 Inspection rules
6.1 Inspection classification
6.1.1 Type inspection
Type inspection items include all items specified in Chapter 4:! , chemical composition, product type should not be inspected during normal production and use. In the following circumstances, a type inspection should be carried out.
When formal production is stopped, raw materials, management (including chemical) or other aspects have major changes, or equipment changes may affect product quality:
b) When full production is stopped, a type inspection should be carried out regularly, in particular once a month:
d) When the inspection result is significantly different from the previous type inspection result:
e) When the national industry management department proposes to conduct a type inspection: 6.1.2 Factory inspection
All items except the inspection density in 4.4 are included in the inspection date, and the inspection date is 3
QB/T1768-2003
6.2 Product batching and sampling rules
6.2.1. Product delivery and sampling inspection. Products of the same specification and batch number delivered at one time are products delivered by a production unit. They should first be inspected by their quality inspection department according to this standard. If they meet this standard and have a product quality inspection certificate, the production site quality inspection certificate shall include: manufacturer name, product name, trademark, standard number, batch number, batch number, quantity mark, production data, etc. The quality control inspection of the received products shall be carried out according to the following provisions within one year. 6.2.2 Sampling inspection
The number of samples required for inspection shall be determined according to the batch size according to Table 2. The receiving parties shall jointly pull the samples from the batch at the delivery location. Table 2 Batch and sample size
Sample size
16--25
91-150
151--503
501--1200
1201 When sampling, fold the sampler into the center of the package into one quarter and collect the sample. Each sample should be transported to the corresponding position. The sample should be quickly collected and added. The total amount of sampling should not be less than 2. The sample should be divided into 1.5 kg according to the quartering method, and packed into three clean and dry containers, and sealed. The label should indicate the product name, product batch number and model number, production unit, sample number, sampling date, and sampling person. The two parties to the delivery shall hold one copy for inspection and the other copy for the delivery party to keep for inspection and storage for three months. 6.3 The inspection results shall be compared with the standard to determine whether they are qualified or not. If one item of the physical and chemical index is unqualified, a new sample of twice the original will be taken for physical inspection: if the re-inspection result is still unqualified, and if the batch of products is not qualified. If the results of the four inspections of the two parties to the delivery are different, if no agreement can be reached, arbitration can be requested, and the final result will be the final result. 7 Marking, packaging, transportation and storage
7.1 Marking
7.1.1 The packaging shall be marked with the following:
a) Product specifications, with or without label: b) State standard number;
Net content:
Name, address and contact number of the production unit, etc.;
7.1.2 The labels (pictures and text) printed on the packaging shall be clear and beautiful, without fading: 1.2 Packaging
Use inner sealed plastic bags for packaging, and the net weight of the packaging shall meet the nominal pressure; 1.3 Transportation
Avoid sun, rain and air conditioning during transportation and handling to avoid damage to the packaging. 7.4 Storage
The product should be stored in a well-protected warehouse. If it is necessary to store it in the open air, the pile should be at least 0 meters above the ground and equipped with a minimum support of more than 1 meter. Cover it with protective clothing to prevent sunlight, moisture and damage. 4
A.1 Test conditions
Appendix A
(Existing Standard Specification for X-ray Diffraction Method)
4A X-ray diffraction product type (X-ray diffraction method) QR/T1768—2003
Cu 20 kV, 25 nV, monochromator with stone pad, scanning speed 4/mim, scanning speed 20-3~40A.2 Sample preparation
Take 18 grams of the product to be tested, put it into a box that has been cooled to 10°C, dry it for 3 hours, and then put it into a constant temperature container with saturated chloride ions at the bottom to fully absorb moisture. 81 A.3 Determination
According to the X-ray diffraction procedure, change the selected test conditions to determine the sample, and obtain the X-ray diffraction spectrum or 2α-d value of the sample:
A.4 Determination
Compare the X-ray diffraction spectrum or 2α-d value with the 11590 slice in the PowerDirections File of the International Union of Technical Diffraction Standards (.lnintcammitteondiffractionstandards). If they match, the sample is determined to be 4A full stone: If only one of the values does not match, the corresponding residual scan type is obtained. QB/T1768-2003
Appendix B
(Normative Appendix)
Foam detergent with 4 Determination of calcium exchange capacity of A zeolite B.1 Determination of exchange capacity of detergent with 4A zeolite Hygroscopic method (mid-cut method) B.1 Principle
The calcium of the element reacts fully with 4A zeolite under certain conditions, and the remaining is indicated by the indicator NN) and the solution is fully determined with ethylenediaminetetraacetic acid disodium (ELXIA). When the pH is greater than 2.5, the calcium (Ca) indicator generates a reddish reaction product (see the reaction formula): When the solution is titrated with FDTA, the calcium ions originally combined with the calcium ion are gradually taken away by EDTA, and the remaining calcium in the solution is removed and gradually separated from the calcium indicator, and the color of the indicator itself changes to indicate that the end point has been reached NN+C→CNN (red).
EDTA+CaNN-→EDTA+N N)
The remaining calcium ions are measured, and the exchange energy is obtained. BT2 reagent
B.1.2.1 Disodium EDTA (GB/T1401), c (EDTA) = U.U1 mol/L. Titration solution GB/60E-2002 4.15 and standard e (ELTA) -0.L mol/L, 10 times the standard titration solution 0.0ImO1/LEDT, if necessary, re-standardize! 1.2.2 Calcium chloride, CaC1 = 0.5mol) Preparation: Weigh 5.6% calcium chloride in water (weigh to 0.001 K: dilute with water to 1000m: b) Calibration: absorb the solution in a transfer tube for 20m: 100m. Keep the plate tightly closed, dilute until the breath is full, then take 20ml of the 250m. piece of sample, add 50ml., 2mL1 of 2.5mol/L sodium hydroxide as a standard indicator, and titrate with the DA standard tide (B.1.2.1) from the alcohol to the color of the standard solution as the end point: the concentration of the calcium chloride standard solution is expressed in grams, and the nuclear formula (B.!) is calculated. GxPx5
Calcium hydroxide (CaCl) standard solution concentration, mol/L: -EDIA standard titration solution [B.1.2.1) number, mol/: ratio -… During calibration, the content of EEIA standard titration solution is as follows: mIB.1.2.3 Sodium hydride (GR/T (29), (NaOIT) = 2.5 mol/T. Weigh 10 grams of sodium hydride and dilute to 1mE: B.1.2.4 Sodium chloride 1GB/9). (NaOIT) -0.5 mol/L weigh 2g of sodium hydride and dilute to 100ml
day.1.2.5 Calcium indicator
day) 2-nitrophenyl- (2-nitrophenyl-4-nitrophenyl-) - Prohibition test) -3-case A-type plate (rotation test of carboxylic acid); D) Ca2PO4 (GB/T1266!:
c) Preparation of calcium indicator: Mix 1 part of the above substance a and 1 part of substance b by pressure: B.1.3 Instruments
Experimental instruments
a) Warm water, dynamic air temperature at (35+1), 6
fixed filter paper: medium speed, 150mm area 150mm×150m: b)
flask, 1000mL
temperature furnace, the whole is automatically controlled at (S00±10) tidal controller, hygrometer, saturated ammonium hydroxide melt (relative humidity about %; stirrer, see Figure B. 1,
burn the ground, 30mL:
T stirrer, filled with glue T end agent.
Method: Material fire to build or human example
Figure R.1 Schematic diagram of stirrer
B.1.4 Test procedure
B.1.4.1 Sample standard
Q/T1766-2003bzxz.net
Use a bottle or a small beaker to take 5~10g of the stone sample and dry it in an oven at 105~110℃ for 2h, then place it in a thermostat[.1.3] and keep it for more than 24 hours for use (during the drying and moisture absorption process, the secret book will not be damaged!), B. 1. 4. 2. Determination of the amount of water to be absorbed: a) Weigh 0.5g of the sample treated with (B.1.41) in the test site of the laboratory, and transfer to two portions of 0.1g. Place them on a fixed moisture-absorbing pad. Take 0.5g of the sample and put it in a filter paper bag, weigh it to 0.1g, and weigh one portion and two portions successively for the determination of calcium exchange capacity. The first portion should be deionized and tested if necessary. The test of calcium exchange capacity and moisture absorption capacity will be determined successively. b) Determination of apparent water absorption: Put the weighed sample [B.1.4.2a>] (covered with a high temperature protection of 800℃ [B.1.3d), and put it into a desiccator LB for 1.3h) in a jar, cool to room temperature, and measure in parallel. Determine the calcium exchange capacity: Pipette 50mL of 0.05mol/L calcium chloride (1.2.2) into 500mL of air, add water and weigh to the mark (or use a 50mL bottle to take 0.05mol/L calcium chloride solution to the mark). 0.05mol/L sodium hydroxide solution (QB/T1768-2003, 1.2.4) is dissolved to a volume of 10.2~10.5. Then transfer this solution into a 1000mL bottle, install a thermometer, add oxalic acid in another bottle, and put it into a constant temperature water bath at 35±1. : Stir at a speed of 700/m2 and the liquid does not fly. When the liquid reaches the controlled temperature, take out the three bottles and put them into the test sample [B.1.4.3a, and then filter it with a 2-layer quantitative paper (or other paper with the same performance). If the concentrated liquid is not clean, filter it again. After that, absorb 50% of the liquid and 250% of the liquid in the whole bottle. Add 2 mL of 2% oxidizing agent [B.1.2.3] and 60 mg~70 mg of calcium indicator B.1.2.S. Titrate with EDTA standard solution B.1.2.1) until the red-blue color is the end point. Record the consumption of DTA standard solution! B.1.5 Calculation of results ||tt| ... %)=m-m100
The mass of the sample before burning,
m2·The mass of the sample after burning, g:
The result is expressed as the average rate to the integer: (B.2)
Precision: Under repeated conditions, the difference between the test results is 5, and the light is not more than 5%.
b4A The calcium cross-linking capacity of the calcium ion is expressed as an integer gram, and is calculated according to the formula (B.3). 100.08(5e10,)
The concentration of the standard EDTA titration solution (B.1.2.2) is mol/L: The concentration of the EDTA standard titration solution (B.1.2.1) is: nwI/L In R.1.41.2c, the product of the standard FTTA titration solution is used! ：ml：Selected mass,
I--calculated in millimeters according to B.1.5?%,%
Carbon and calcium are generally required to be expressed as integers (B.3)
Precise determination: The difference between the two test results obtained under five conditions should not exceed 3CC0-10, with the premise that the washing amount should not exceed 5% on a 3macO-dry basis. B.1.6 Notes
a) The weighing time of parallel selected products should be as close as possible; b) The time for placing the detergent should not be too long.
H.2 Determination of calcium exchange capacity of 4A zeolite for detergents Ignition loss method (fast method) B. 2. T Principle
Na in the CaO2 solution is replaced by 4A, and the amount of aluminum dissolved is recorded under the control gas recording device. The remaining DIA-Cu·PAN indicator indicates that the calcium carbonate (Ca2O3) reacts with DTA-Cu·PAN to form a purple complex. When the EDTA droplets are mixed with this solution, the calcium carbonate originally complexed with the indicator is partially separated by EDTA. For each batch of newly purchased calcium oxide (2.1.2.2 or newly prepared B.1.2.4), the pH meter is used to measure the state of the solution to 0.5 500 mml of calcium hydroxide solution, the amount of 0.5 m/s sodium hydroxide solution required when the H is 10.2·n.5, and then use this batch of solution to determine the H. The same commercially available 0.5 mDl solution can be used to test the H. After the reaction, the free LYIA solution is released, indicating that the solution is full of calcium, which means that the end point has been reached: the residual calcium is measured according to the standard EDTA content: the boiling point calcium exchange capacity can be calculated. B. 2.2 Test data
B.2.2.1 Hydrogen flushing solution, PH-1U
a) Ammonium hydroxide (GB/T658):
h) GT61
Preparation of hydrogen flushing solution: weigh 54% of ammonium hydroxide, dissolve in water: transfer into a 120ml container, add 350mL of hydrogen, and mix with a small amount of dilution.
A.2.2.2 Ammonium hydroxide GRT629! (NAOFT) = 1 moi/1. Weigh 4.0 g of sodium hydroxide and add 100 ml of solution: B.2.2.3 Ethyl tetraethyl phthalate (EDTA): (GB/T140I, (ETA = 0.11 mal/T.) Prepare the quasi-titration solution according to RT version 1-2, 4.15 and calibrate TDTA = 0.01 mol/L. Prepare the quasi-titration solution according to RT version 1-2, 4.15 and calibrate TDTA = 0.01 mol/L. Use the standard titration solution of U.0 MoI/EDTA for clinical use. B.2.2.4 Ethyl tetraethyl phthalate (EDTA-Cu) solution, 0.01 mol/L l/L transfer image (CuSO5H0) (CR/T665) 2.4968: 1 mL of TDTA standard solution (B.2.2.3) was transferred to 1 [guest, and the ratio of A to the solution was added until the 1.5 t, and then inserted. B.2.2.5 Calcium chloride, c (Cacl) - 0.05 mol/L standard solution, 5.6 g of anhydrous calcium hydroxide (the weight was reduced to 1.0), and the water content was adjusted to 100 ml/day. 2.2.61-: 2-chloro-2-nitrogen powder (AK) (HGT3.J08), 1.1 ethyl acetate solution.9. 2. 3 Receiver
inform the industrial room positioner and
a! Requirement, energy end (35±):
b fixed micro, medium speed: 150mm or 150mm150mmc) two-mouth environment bottle, 100iml
d) stirrer, lead D.1.
B. 2. 4 Blank titration
Take 0.05ml/1.50ml of the chemical (R.2.2.5) and 50ml of 1mol/1 sodium hydroxide (B.2.2.2) in a plate, dilute to 1mol/1 sodium hydroxide (B.2.2.2) with water, mix well, transfer 50ml of the solution to a 300ml flask, add 1mL of ethylamine tetraacetic acid solution (B.2.2.4), 3 bags of PAN indicator (B.2.2.6), 15ml of ammonia solution (B2.2.1), HFT-TA standard titration solution (R.2.2.3), and titrate to the endpoint of liquid-to-water ratio. Record the external product (P) of the EDTA standard titration solution. B. 2. 5 Determination
B. 2. 5. 1 Weigh the sample
and carry out the determination of average calcination amount in the following step. Weigh 0.5 mg of the sample into the filter bag and add two portions in parallel. First, take the necessary steps: B.2.5.2 Titration
and take 0.05 mol/L calcium hydroxide solution (B, 2.2.5) with a pipette. 50 ml + 500 ml. Add the diluted solution to or above, add the hydrogen peroxide (B, 2.2.2) to the standard concentration (0.5 ± 0.1), and add the source into a 1000 ml flask. Place the flask in a (35 ± 1) t cooling water bath. Adjust the rotation speed to 6 [B.2.3d) 00r/m~700rnin, after constant humidity, put the test sample (R.2.5.1) into the environment, react for 20m, filter the mixture with fixed combustion filter paper (or other paper with equal performance), fill the initial part, the solution becomes transparent (such as secretion, gradually remove the residue), use a liquid pipette to absorb 300ml of the sediment into a conical bottle, add water until the medicine accumulates 100L, add 0.01ol/1EDTA-Cu float (B.2.2.4) 1mL, add a small amount of PA (R.2.2.6), nitrogen flushing liquid (month.2.2.1>15m[.month TDTA standard titration solution (B.2.2.3) for the final color wave, and the volume of the micro-solution () is determined by the approved process. Qn/T1768-2003
The conversion capacity of 4A is expressed as grams of anhydrous boiling point and grams of calcium carbonate. The concentration of EDTA standard solution is calculated by formula (D.4): 100.08×10×ex(,-V.)
non×(1 -)
, OLL: volume of empty H2O EDTA standard solution in titration, H3: volume of FTTA standard solution in test titration, mL test mass,
the average weight of 4A determined in 5.1.4, %, %: calcium carbonate content, mg/mmal
the results are expressed as arithmetic mean integers. (Month.4)
Density: The stem value of the rice obtained in two independent tests under the crown of the year is not greater than 3maC0/g·ten base, with the premise that the stem value of 3mgCa/g-stem does not exceed 5.R.2.6. Notes
a) Each batch of lamps should be prepared with standard calcium hydroxide solution (B.2.2.5) or newly prepared sodium hydroxide solution.
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