T 665 cm-02

SUGGESTED MEHTOD 1965 OFFICIAL TEST METHOD 1983 REVISED 1989 REVISED 1993 REVISED 2002 2002 TAPPI The information and data contained in this document were prepared by a technical committee of the Association. The committee and the Association assume no liability or responsibility in connection with the use of such information or data, including but not limited to any liability under patent, copyright, or trade secret laws. The user is responsible for determining that this document is the most recent edition published.

CAUTION: This Test Method may include safety precautions which are believed to be appropriate at the time of publication of the method. The intent of these is to alert the user of the method to safety issues related to such use. The user is responsible for determining that the safety precautions are complete and are appropriate to their use of the method, and for ensuring that suitable safety practices have not changed since publication of the method. This method may require the use, disposal, or both, of chemicals which may present serious health hazards to humans. Procedures for the handling of such substances are set forth on Material Safety Data Sheets which must be developed by all manufacturers and importers of potentially hazardous chemicals and maintained by all distributors of potentially hazardous chemicals. Prior to the use of this method, the user must determine whether any of the chemicals to be used or disposed of are potentially hazardous and, if so, must follow strictly the procedures specified by both the manufacturer, as well as local, state, and federal authorities for safe use and disposal of these chemicals.

Analysis of talc
1. Scope These methods cover the identification and the chemical analysis of talc. 2. Summary

Procedures are given for the following: identification by X-ray diffraction, loss on ignition, silicon dioxide, R2O3 group, calcium oxide, and magnesium oxide. 3. Significance

3.1 Pure talc is a hydrous magnesium silicate, Mg3Si4O10(OH)2, with a theoretical chemical composition of 31.7% MgO, 63.5% SiO2, and 4.8% H2O. Unground it may be white, greenish, gray, or almost black, depending on the impurities present, but when ground, talc is normally white to grayish white. 3.2 Commercial talc is rarely pure, containing at least one of the following impurities: a-quartz, tremolite, kaolinite, serpentine, chlorite, muscovite, calcite, dolomite, magnesite, and asbestos (chrysotile). Commercial talc may, in fact, contain less talc than impurities. 4. Apparatus, reagents, and materials Any specialized apparatus, materials, and necessary reagents are included in the appropriate sections of All chemicals should be of reagent grade or better. Water used in the procedure should be distilled or deionized. A complete reagent blank run along with the sample is recommended, if the reagents are of suspect All weighings are to be performed on an analytical balance and recorded to four decimal places.

4.1 the procedure. 4.2 4.3 4.4 purity. 4.5

Approved by the Standard Specific Interest Group for this Test Method TAPPI

T 665 cm-02

Analysis of talc

5.

Sampling and test specimen

From each test unit of at least 400 g obtained in accordance with T 400 Sampling and Accepting a Single Lot of Paper, Paperboard, Fiberboard, or Related Product, grind approximately a 10-g specimen to -325 mesh (<44 m) for Xray diffraction. 6. Procedures 6.1
NOTE 1:

Identification by X-ray diffraction

6.1.1 6.1.2 6.1.3 pattern.

Apparatus: standard X-ray diffraction system. Prepare the specimen of the ground talc as described by Klug and Alexander (1). Obtain the diffraction pattern (1) of the specimen and calculate the d-spacings of the sample from the
Fang and Bloss (2) provide 2q to d-spacing conversion tables.

6.1.4 For identification purposes, Table 1 contains a listing of the major d-spacings for talc and the common mineral contaminants mentioned in 3.2. 6.2 Loss on ignition 6.2.1 Accurately weigh approximately 1 g of the sample that has been dried for 1h at 105C into a tared crucible. Ignite to constant weight starting at 400C and gradually increasing to 1000C. One hour at full heat is sufficient. 6.2.2 Allow the crucible and its contents to cool to ambient temperature, cool in a desiccator, and weigh. 6.2.3 Calculation: Loss of ignition, % = (weight loss, g)(100%) / (sample weight, g) 6.3 Silicon dioxide 6.3.1 Materials: platinum crucible and close fitting lid. 6.3.2 Reagents 6.3.2.1 Sodium carbonate (Na2CO3), powder. 6.3.2.2 Hydrochloric acid (HCl), concentrated (sp. gr. 1.19). 6.3.2.3 Hydrochloric acid, 1 + 20 (one part of HCl with sp. gr. of 1.19 and 20 parts water). 6.3.2.4 Sulfuric acid, 1 + 1 (one part of concentrated H2SO4 and 1 part water. 6.3.2.5 Hydrofluoric acid (HF), 48%. 6.3.3 Accurately weigh approximately 0.5 g of the sample into a platinum crucible, mix 5 g of Na 2CO3 into the same crucible, and cover with a close fitting platinum lid. Heat in a muffle furnace starting at 500C for 10 min and gradually increase the temperature to 1100C to obtain a clear, quiet fusion. Generally 60 min of strong heating is sufficient. 6.3.4 Allow the crucible and melt to cool to ambient temperature and place the entire crucible and lid into a 600-mL porcelain casserole containing 200 mL of water. Boil until the melt disintegrates. 6.3.5 Remove the crucible and lid with platinum-tipped tongs and carefully rinse out any adhering particles into the same casserole. Cover the casserole with a watch glass and carefully acidify the contents by slowly pouring concentrated HCl in the spout and down the sides of the casserole while maintaining a slow swirling motion.
NOTE 3: Care must be taken to avoid losses due to spattering caused by the evolved CO2.

6.3.6 Add 30 mL of concentrated HCl in excess and evaporate to dryness on a steam bath. When dry and no odor of HCl can be detected, wash down the sides of the casserole, add 150 mL of water, and bring to a slow boil. Filter while hot through low-ash, fine-porosity filter paper (Whatman No. 44 or equivalent). Wash the filter paper at least five times with hot 1 + 20 HCl following by hot water washing until the filtrate is acid free. 6.3.7 Reevaporate the filtrate; when dry, dilute to 150 mL as before and filter in the same paper. Wash well until acid free. Retain the filtrate for determination of R2O3 group.

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T 665 cm-02

6.3.8 Transfer the filter paper and its contents to a platinum crucible, char and burn the filter paper gently to avoid losses, and ignite the residue at 850C for l h. Cool in a desiccator and quickly weigh (W1). 6.3.9 Moisten the residue with 1 + 1 H2SO4, fill the crucible half way with 48% HF, and evaporate to dryness on a steam bath. 6.3.10 Repeat 6.3.9. When the residue is dry, ignite at 850C for l h, cool in a desiccator, and quickly weigh (W2).
NOTE 4: To be absolutely certain that all of the silica has been volatized, repeat 6.3.9 and 6.3.10 until a constant weight is attained.

Calculation: SiO2, % = (W1 - W2) (100%) / (sample weight, g) 6.4 Ammonium hydroxide group (R2O3) 6.4.1 Reagents 6.4.1.1 Potassium pyrosulfate, K2S2O7 6.4.1.2 Hydrogen peroxide, H2O2, 2% solution. 6.4.1.3 Methyl red indicator solution 6.4.1.4 Ammonium hydroxide, NH4OH, concentrated (sp. gr. 0.90). 6.4.1.5 Ammonium chloride, NH4Cl, 2% solution. 6.4.2 If any residue remains in the crucible from the silicon dioxide determination, fuse with a small amount of K2S2O7, leach the fusion from the crucible with water, and combine with the filtrate from 6.3.7. 6.4.3 Add 5 mL of 2% H2O2 to the filtrate, bring to a boil and maintain boiling for 10 min. Remove from heat, neutralize while hot with concentrated NH4OH to a methyl red end point, and add 2-3 drops in excess. Continue heating on a low plate until precipitate coagulates. 6.4.4 Filter the solution while hot through low-ash, medium-porosity filter paper and wash at least four times with hot 2% NH4Cl.
NOTE 5: If increased accuracy is desired, the precipitate may be redissolved in hot 1 + 3 HCl and reprecipitated as described in 6.4.3.

6.3.11

6.4.5 Transfer the filter paper and its contents to a tared crucible, dry and char the paper, and ignite carefully to avoid reduction to a constant weight at 1000C. Cool in a desiccator and weigh the residue as R2O3. 6.4.6 Calculation: R2O3, % = (residue weight, g) (100%) / (sample weight, g) 6.5 Calcium oxide 6.5.1 Reagents 6.5.1.1 Potassium hydroxide, KOH, 20% solution. 6.5.1.2 Ascorbic acid, powder. 6.5.1.3 Hydroxynaphthol blue 6.5.1.4 0.005M disodium ethylene dinitrilotetraacetic acid dihydrate (EDTA), standard volumetric solution, standardize vs. primary standard grade calcium carbonate (CaCO3). 6.5.2 Repeat 6.3.3 through 6.3.6, catching the filtrate in a 500-mL volumetric flask. Dilute to the mark with water and mix. Use for calcium oxide and magnesium oxide (6.6) determinations. 6.5.3 Remove a 50-mL aliquot, dilute to 300 mL, and adjust the pH to 12.0-12.5 with potassium hydroxide solution. 6.5.4 Add 50-100 mg of ascorbic acid, 25-50 mg of hydroxynaphthol blue indicator, and titrate with 0.005M EDTA to a deep blue end point. 6.5.5 Calculation: CaO, % = (volume 0.005M EDTA, mL) (CaO titer, g/mL) (500 mL) (100%) / (sample weight, g) (50 mL) 6.6 Magnesium oxide 6.6.1 Reagents 6.6.1.1 Ammonia buffer, dissolve 66 g NH4Cl in 300 mL water, add 560 mL NH4OH (sp. gr. 0.90), and dilute to 1000 mL. 6.6.1.2 Calmagite indicator 6.6.1.3 0.05M EDTA, standardize vs. primary standard grade calcium carbonate (CaCO3). 6.6.2 Remove a 50-mL aliquot from the solution prepared in 6.5.2, dilute to 300 mL and adjust the pH to 10.010.5 with ammonia buffer. 6.6.3 Add exactly the amount of 0.005M EDTA equivalent to the calcium oxide as determined in 6.5.4.

T 665 cm-02 6.6.4 6.6.5 7. Report

Analysis of talc Using calmagite indicator, titrate with 0.05M EDTA to a deep blue end point. Calculation MgO, % = (volume 0.05M EDTA, mL) (MgO titer, g/mL) (500 mL) (100%) (sample weight, g) (50 mL)

7.1 Identification by X-ray diffraction: report the presence of all minerals identified by name. If the presence of an unidentified phase(s) is suspected, this should be included in the report. 7.2 Report all chemical analysis results in percent, based on the as received weight of the talc, to a maximum of three significant figures. 8. Precision Relative 5% 5% 15% 5% 5% Absolute 0.3% 1.9% 0.3% 0.1% 1.7%

Repeatability: Loss on ignition Silicon dioxide R2O3 group Calcium oxide Magnesium oxide
NOTE 6:

Use whichever value is greater. Values were obtained using a talc sample of the following composition: loss on ignition = 5.4%; silicon dioxide = 60.4%; R2O3 group = 2.3%; calcium oxide = 0.5%; magnesium oxide = 31.4%.

9.

Keywords

Talc, X-ray diffraction, Loss on ignition, Magnesium silicate, Silica, Ammonium hydroxide, Calcium oxide, Magnesium oxide 10. Additional information

10.1 Effective date of issue: April 24, 2002. 10.2 This revision now contains a statement of significance, identification by X-ray diffraction, and references. The procedures themselves have been updated and a precision statement has been added. Tests for pH, brightness, free moisture, and screen residue have been deleted as they are now separate TAPPI methods. The test for alum demand has been deleted. 10.3 Related methods: TAPPI T 667 pH of Fillers and Pigment Slurries, TAPPI T 646 Brightness of Clay and Other Mineral Pigments (O-45 Directional), TAPPI T 534 Diffuse Blue Reflectance Factor of Clay and Mineral Pigment, UM 655 Particle Size Distribution of Pigments and Fillers, TAPPI T 657 Sampling of Fillers and Pigments, TAPPI T 671 Free Moisture in Fillers and Pigments, TAPPI T 681 Screen Residue of Paper Coating Clays and Related Pigments (High-Speed Mixer Method), and ASTM D-717 Analysis of Magnesium Silicate Pigments. References 1. 2. 3. Klug and Alexander, X-ray Diffraction Procedures for Polycrystalline and Amorphous Materials, John Wiley and Sons, New York, 1974, Second Edition, pp. 372-373. Fand and Bloss, X-ray Diffraction Tables, Southern Illinois University Press, 1966. Berry, L. G., ed., Power Diffraction File, Joint Committee on Powder Diffraction Standards (JCPDS); Volume: Inorganic, 1976.

5 / Analysis of talc

T 665 cm-02

Table 1. Mineral Talc a-Quartz Tremolite Kaolinite Serpentine Chlorite Muscovite Calcite Dolomite Magnesite Asbestos

X-ray diffraction data for identification (3) Major d-spacings 3 forms of Talc are listed by (JCPDS) 3.34x 4.264 1.822 8.38x 3.12x 2.719 7.17x 3.588 4.376 6 forms are listed by JCPDS 32 forms are listed by JCPDS 5 forms are listed by JCPDS 3.04x 2.292 2.102 2.89x 2.193 1.793 2.74x 2.104 1.703 7.38x 4.557 3.663 2.461 3.278 4.195 2.281 2.815 2.505

1.912 2.022 2.502 2.453

1.882 2.411 1.941 1.542

Your comments and suggestions on this procedure are earnestly requested and should be sent to the TAPPI Director of Quality and Standards. g