PIA-TEST METHOD-2611D-2014 NONFIBROUS MATERIALS IN COTTON ENZYME METHOD.pdf

1、 The following commercial specification is adopted from the military document. Revision A includes all known accepted revisions, amendments, notices, and Department of Defense (DoD) engineering changes previously developed for this item. Revisions B and forward include changes adopted to reflect tec

2、hnology and design evolution. NONFIBROUS MATERIALS IN COTTON, ENZYME METHOD The Parachute Industry Association makes this document available for use by Industry and Government organizations that wish to apply this specification to their products. 1. SCOPE 1.1 This method is intended for determining,

3、 in cotton or cellulosic mixture yarns or cloths, the amount of sizing, finishing, and other nonfibrous materials, such as oils, fats, waxes, minerals, and other materials which will be removed or determined by chloroform and/or water extraction, hydrolized by enzyme action, or remain as inorganic m

4、aterial after exposure to high temperatures. Although this method is intended for the determination of nonfibrous materials in cellulosic textiles, it may be used for determining the extractable and nonfibrous materials content of certain noncellulosic textiles, as specified in the applicable end it

5、em specification or procurement document. 1.2 This method is not applicable to the determination of the amount of permanent types of finishes, such as urea condensates, melamine condensates, and substantive or organic finished, or to finishes that are volatile at 230F (110C). 2. TEST SPECIMEN 2.1 Th

6、e specimen shall be approximately 10 g of the material undergoing test. Care should be taken in the preparation and subsequent handling of the specimen, so that loss of material will not occur during test. If the material undergoing test is woven or knitted cloth, the specimen should be cut on the b

7、ias and have loose fibers and yarns removed. 2.1.1 When total ash is required, an additional 10 g specimen is required for evaluation. 3. NUMBER OF DETERMINATIONS 3.1 Unless otherwise specified in the procurement document, two specimens shall be tested from each sample unit. 4. APPARATUS AND REAGENT

8、S DISTRIBUTION STATEMENT: All Rights Reserved. No Part of this publication may be reproduced without prior written permission from Parachute Industry Association. Additional copies may be purchased on-line from PIA Specifications and Products: . PIA-TEST METHOD-2611D 04 June 2014 Superseding PIA-TES

9、T METHOD-2611C 24 May 2010 Copyright Protected: Do Not Copy!PIA-TEST METHOD-2611D 4.1 Apparatus. 4.1.1 Analytical balance. Analytical balance capable of weighing accurately to 0.001 g. 4.1.2 Weighing bottle with ground glass cover. 4.1.3 Soxhlet extraction apparatus. 4.1.4 Muffle furnace. 4.1.5 Stai

10、nless steel sieve. 80 to 100 mesh or equivalent. 4.1.6 Desiccator with suitable desiccant. Anhydrous calcium sulfate or anhydrous calcium chloride have been found suitable. 4.2 Reagents. 4.2.1 Chloroform, U.S.P. 4.2.2 Iodine solution. An approximate 0.01N stock solution of iodine (0.13 g of iodine a

11、nd 2.6 g of KI in 100 ml of water) may be prepared, and a portion of this diluted to a pale yellow color (about 0.001N) each time a test for starch is made. 4.2.3 Amylolytic and proteolytic enzyme mixture (see 7.1). 4.2.4 Millons reagent. Millons reagent shall be prepared by adding 25 g (17.6 ml) co

12、ncentrated nitric acid (sp. gr. 1.42) to 25 g (1.84 ml) of mercury under a hood. Upon completion of the reaction, the solution shall be diluted by adding in equal volumes of distilled water. 5. PROCEDURE 5.1 Weight of dry specimen. The specimen shall be placed in a weighing bottle and dried in an ov

13、en at a temperature of 221 to 230 F (105 to 110C), cooled in a desiccator, and weighed to the nearest 0.001 g. This is the “Weight of the dry specimen” and in the calculation of results is indicated as “0”. 5.2 Chloroform-soluble material. The dried specimen from 5.1 shall be extracted with chlorofo

14、rm for a minimum of 20 extractions in Soxhlet extractor. If the weight of the chloroform-extractable matter is required, the extract shall be dried to constant weight in a tared container at a temperature of 174 to 178F (79 to 81C), cooled in a desiccator, and weighed to the nearest 0.001 g. This is

15、 the “Weight of chloroform-soluble material” and in the calculation of results is indicated as “C”. 5.3 Water-soluble material. The specimen from 5.2 shall be placed in a Soxhlet extractor with distilled water and subjected to a minimum of 10 extractions. If the weight of the material is required, t

16、he extract shall be dried to constant weight in a tared container at a temperature of 212 to 215F (100 to 102C), cooled in a desiccator, and weighed to the nearest 0.001 g. This is the “Weight of the water soluble material”, and in the calculation of results is indicated as “W”. Page 2 of 5 Copyrigh

17、t Protected: Do Not Copy!PIA-TEST METHOD-2611D Chloroform and water extractions must be performed in determining starch and protein content. However, the determination for weight of extract, and calculations involved, may be omitted when the exact amounts of water and chloroform-soluble material are

18、 not required. 5.4 Weight of desized specimen. The specimen from 5.3 shall then be immersed in a suitable aqueous enzyme solution containing both amylolytic and proteolytic components at the concentrations, liquid to fabric ratio, temperature, and length of time required to remove the finish as reco

19、mmended by the manufacturer of the enzymes. The specimen shall be removed from the enzyme solution on a sieve, squeezed and rinsed to remove the enzyme solution. This shall be done by alternately squeezing and rinsing the specimen in a minimum of 12 successive baths of distilled water at 154 to 165F

20、 (68 to 74 C). After rinsing, the specimen shall be spot-tested for the presence of starch with the iodine solution and for protein with Millons reagent. The presence of starch is indicated by a blue coloration and the presence of protein by a red coloration. If either test is positive, repeat the e

21、nzyme treatment with the required rinsing until the spot-tests are negative. If additional treatments are required, the specimen shall be thoroughly rinsed before repeating the enzyme treatment. After the enzyme solutions have been completely removed from the specimen, the specimen shall be dried to

22、 constant weight (0.001 g) as described in 5.2. This is the “Weight of the desized specimens” and in the calculation of results is indicated as “S”. 5.5 Residual ash. The desized specimen from 5.4 shall be ashed to constant weight at a temperature of 1112 to l202F (600 to 650C) in a tared porcelain

23、crucible employing a muffle furnace. After ashing, the ashed specimen and the crucible shall be placed in a desiccator, cooled, then removed and weighed immediately to the nearest 0.001 g. The weight of the tared crucible shall be subtracted from the total weight to give the “Weight of residual ash”

24、, which in the calculation of results is indicated as “R”. 5.6 Total ash (inorganic material). The specimen from 5.1 shall be ashed to constant weight at a temperature specimen shall be cooled in a desiccator and weighed to the nearest 0.001 g. This is the “Weight of the total ash” and in the calcul

25、ation of results is indicated as “A”. 5.7 Calculation of results. 5.7.1 The results shall be based on the weight of the dry specimen and shall be calculated to the nearest 0.1 percent using the following formulas: Chloroform-soluble material only C x 100 O Chloroform-soluble and water-soluble C + W

26、x 100 material only O Water-soluble material W x 100 O Starch and protein content excluding O - S - W - C x 100 chloroform-soluble and water-soluble O material Starch and protein content including O - S x 100 Page 3 of 5 Copyright Protected: Do Not Copy!PIA-TEST METHOD-2611D chloroform-soluble and w

27、ater-soluble O material Starch and protein content including O - S - W x 100 chloroform-soluble material O Starch and protein content including O - S - C x 100 water-soluble material O Residual ash only R x 100 O Total ash only A x 100 O Total sizing, finishing, and other O - S + R x 100 non-fibrous

28、 material content O Where: O = Weight of original dry specimen, g (5.1) C = Weight of chloroform-soluble material, g (5.2) W = Weight of water-soluble material, g (5.3) S = Weight of desized specimen, g (5.4) R = Weight of residual ash, g (5.5) A = Weight of total ash, g (5.6) 6. REPORT 6.1 The chlo

29、roform-soluble material, water-soluble material, starch and protein content, total ash, residual ash, and total sizing, finishing, and other non-fibrous material of the sample unit shall be the average of the results obtained from the specimens tested and shall be reported to the nearest 0.1 percent

30、. 7. NOTES 7.1 The proteolytic and amylolytic enzymes used for removal of starch and protein compounds can be obtained from most chemical supply houses. * Notice: This document has been adopted from the original Mil-Spec of the same number and is being maintained as a commercial specification by the

31、 Parachute Industry Association. Orders, inquires and comments should be addressed to PIA, Specification Committee Via e-mail at: or to our website at: . Page 4 of 5 Copyright Protected: Do Not Copy!PIA-TEST METHOD-2611D Copyright 2004-2014 Parachute Industry Association. Disclaimer: This document

32、 is published by the PIA to provide technical and engineering standards that can be used for reference by all those who may benefit from them. The use of this document is entirely voluntary, and its applicability and suitability for any particular use, including any patent or trademark infringement

33、arising there from, is the sole responsibility of the user. The original Government document was scanned. The PIA reviews each technical publication periodically, at which time it may be reaffirmed, revised, or canceled. The PIA invites your written comments and suggestions. Page 5 of 5 Copyright Protected: Do Not Copy!