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Analytical Letters
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Application of Improved Azomethine-H Method to the Determination of Boron in Soils and Plants
Matt K. John , Hong H Chuah
b a a a b a

& John H. Neufeld

Science Policy Branch, Environment Canada, Ottawa, Ontario, Canada

b

Soil and Feed Testing Laboratory, Field Crops Branch, British Columbia, Department of Agriculture, Kelowna, British Columbia, Canada Available online: 05 Dec 2006

To cite this article: Matt K. John, Hong H Chuah & John H. Neufeld (1975): Application of Improved Azomethine-H Method to the Determination of Boron in Soils and Plants, Analytical Letters, 8:8, 559-568 To link to this article: http://dx.doi.org/10.1080/00032717508058240

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The publisher does not give any warranty express or implied or make any representation that the contents will be complete or accurate or up to date. The accuracy of any instructions, formulae, and drug doses should be independently verified with primary sources. The publisher shall not be liable for any loss, actions, claims, proceedings, demand, or costs or damages whatsoever or howsoever caused arising directly or indirectly in connection with or arising out of the use of this material.

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ANALYTICAL LETTERS, 8(8), 559-568 (1975)

APPLICATION OF IMPROVED AZOKliTHINE-H

METHOD TO THE DETERMINATION

OF BORON I N SOILS AND PLANTS

KEY WOWS: boron d e t e r m i n a t i o n , i o n i n t e r f e r e n c e , s o i l e x t r a c t , p l a n t e x t r a c t , sewage e f f l u e n t , sewage s l u d g e

Matt K. J o h n , Hong H , Chuah

and Jo h n H. Neufeld

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S c i e n c e P o l i c y Branch, Environment Canada, Ottawa, O n t a r i o , Canada

AbSTMCT

An improved c o l o r i m e t r i c method f o r t h e d e t e r m i n a t i o n of boron was

d e v e l o p e d by i n v e s t i g a t i n g t h e e f f e c t s of t e m p e r a t u r e , t i m e , r e a g e n t c o n c e n t r a t i o n and c o m p o s i t i o n of t h e r e a c t i o n m i x t u r e on coloiir developnierit w i t h azomethine-11.

Anong 15 i o n s s t u d i e d , o n l y f l u o r i d e ,

aluminum, f e r r i c and c u p r i c i o n s i n t e r f e r e d w i t h c o l o u r d e v e l o p n e n t a t below 1 0 , 0 0 0 ppm i n sample a l i q u o t . Tolerable concentrations f o r these

i o n s were 5,000 ppm f l u o r i d e , 3.000 ppm aluminum, 2,500 ppm c u p r i c and 200 ppzi f e r r i c i o n .

The method accourited f o r hnown a d d i t i o n s of b o r o n

t o n o r n a l h y d r o c h l o r i c a c i d e x t r a c t of p l a n t material, t o h o t w a t e r e x t r a c t of s o i l and t o e f f l u e n t . Boron u e t e r n i n a t i o n s i n t h e s e samples

a n a sewage s l u u g e e x t r a c t were in c l o s e agreement w i t h r e s u l t s o b t a i n e d by t h e c a r n i n e method. The proposed azometliine-1 method was found

a d v a n t a g e o u s s i n c e use of c o n c e r . t r a t e u s u l p h u r i c a c i d i s a v o i d e d and

smaller v a r i a t i o n s i n r e s u l t s

and s u p e r i o r precision a r e o b t a i n e d .

559
Copyright 0 1975 by Marcel Dekker, Inc. All Rignts Reserved Neither this work nor any part may be reproduced or transmitted in any form or by any means, electronic or mechanical, including photocopying, microfilming, and recording, or by any information storage and retrieval system, without permission in writing from the publisher.

560 INTRODUCTION

JOHN, CHUAH, AND NEUFELD

Rapid and r e l i a b l e boron d e t e r m i n a t i o n s in s o i l s and p l a n t s a r e r e q u i r e d f o r d i a g n o s t i c and r e s e a r c h p u r p o s e s .

A c o l o r i m e t r i c method

employing a ~ o m e t h i n e - H ~ *was ~a d a p t e d t o d e t e r m i n e boron i n a c i d i c ~ sodium a c e t a t e e x t r a c t s and s u l p h u r i c a c i d d i g e ~ t s . However, more ~ i n f o r m a t i o n i s needed t o assess t h e methods p r e c i s i o n and a d a p t a b i l i t y t o o t h e r commonly used e x t r a c t i o n o r d i g e s t i o n p r o c e d u r e s . Factors

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a f f e c t i n g c o l o u r d e v e l o p m e n t , t o l e r a n c e t o ionic i n t e r f e r e n c e and a p p l i c a t i o n t o soil and p l a n t a n a l y s i s were s t u d i e d .

MATERIALS AND METHOUS

Reagent s U n l e s s s p e c i f i e d o t h e r w i s e , r e a g e n t s were p r e p a r e d a s f o l l o w s :

1. B u f f e r masking s o l u t i o n was p r e p a r e d by d i s s o l v i n g 250 g of ammonium

a c e t a t e and 15 g oL ethylenedinitrilo-tetraacetic a c i d d i s o d i u m s a l t (i.e., d i s o d i u m e t h y l e n e d i a m i n e tetraacetate, EDTA d i s o d i u m s a l t ) i n

400 ml of d e i o n i z e d d i s t i l l e d w a t e r and s l o w l y a d d i n g 1 2 5 m l of glacial acetic acid. 2. Azomethine-H azomethine-H6 r e a g e n t was p r e p a r e d by d i s s o l v i n g 0 . 4 5 g of

i n 100 m l of 11 L - a s c o r b i a a c i d s o l u t i o n .

Fresh reagent

was p r e p a r e d e a c h week and s t o r e d i n a r e f r i g e r a t o r .

3.
A s t o c h s o l u t i o n c o n t a i n i n g 20 ppm b o r o n was p r e p a r e d by d i s s o l v i n g 0.1143 g of b o r i c a c i d i n one l i t e r of w a t e r . Standards containing

0 . 5 t o 8 ppm boron were p r e p a r e d by d i l u t i n g s t o c k s o l u t i o n w i t h water o r a p p r o p r i a t e extractant s o l u t i o n .

Sample P r e p a r a t i o n The above-ground p o r t l o n of a l f a l f a (Medicago s a t i v a L.) p l a n t s was i n t e r i o r , oven-dried

c o l l e c t e d from a f i e l d i n B r i t i s h Columbias (B.C.)

am ground.

One-gram s a m p l e s were d r y a s h e d f o r 8 hr a t 55OoC and t a k e n

BORON IN S O U S AND PLANTS

up i n 5 o l of normal h y d r o c h l o r i c a c i d . E x t r a c t s were d e c o l o r i z e d by

561

adding a c t i v a t e d c h a r c o a l , f i l t e r e d through Whatman No. 42 p a p e r and c o l l e c t e d i n acid-weathered f u n n e l t u b e s . S u r f a c e samples of Monroe and Ladner s o i l s were c o l l e c t e d from cultivated fields i n B.C.'s 20-mesh. Lower F r a s e r V a l l e y , a i r - d r i e d and c r u s h e d t o

Five-gram.samples were e x t r a c t e d w i t h 10 m l of h o t water f o r 5 technique described earlier.

niin u s i n g a batch-handling

'

Extracts were

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d e c o l o r i z e d and f i l t e r e d . E f f l u e n t from a m u n i c i p a l sewage p l a n t a t Kelowna, B.C. was c o l l e c t e d a f t e r secondary t r e a t m e n t .

A p o r t i o n was c o n c e n t r a t e d by b o i l i n g o f f

water.
Sewage s l u d g e was o b t a i n e d from a t r e a t m e n t p l a n t t h a t s e r v e s m e t r o p o l i t a n Vancouver, B.C., a i r - d r i e d and ground. llot water e x t r a c t s

were p r e p a r e d as d e s c r i b e d f o r soils.
Deterciination of Boron

Unless s p e c i f i e d o t h e r w i s e , 1 m l of b l a n k , boron s t a n d a r d

OK

sample

s o l u t i o n was p i p e t t e d i n t o a 15-ml polypropylene t u b e and 2 m l of b u f f e r

GIasking s o l u t i o n were added.

The c o n t e n t s of t h e t u b e were mixed, u s i n g Two m l of azomethine-H r e a g e n t were added.

a portable e l e c t r i c a l stirrer.

The r e a c t i o n m i x t u r e was a g a i n s t i r r e d thoroughly and. t h e n allowed t o s t a n d a t room t e m p e r a t u r e f o r 30 n i n . Absorbance a t 420nm was measured The 10-cm r e f e r e n c e and

w i t h a Beckman, Noael D B , s p e c t r o p h o t o m e t e r .

saniple c u v e t t e s were maintained a t room t e m p e r a t u r e by c i r c u l a t i n g water through t h e sample compartment jacl,et. D u p l i c a t e d e t e r m i n a t i o u s of boron i n 4 r e p l i c a t e s of e a c h sample s o l u t i o n were conducted by t h e proposed azomethine-H method and by t h e carmine metliocr d e s c r i b e d by Hatcher and Wilcox. obtaineci by tile two methods were compared.

The r e s u l t s and p r e c i s i o n

562
IUiSULTS APlLl

JOHN, CHUM, AND NEUFELD

1)IscussIoIu
complex formed w i t h t h e 2 ppm

Absorbance by tlie b o r i c acid-azometLinc

boron s t a n d a r d was mxinium a t 410 t o 4 2 0 n m b u t d e c l i n e d 10% a t 430-e The 42bnm wavelength was selected. Although a l i q u o t s i z e v a r i e a from 0 . 2 t o 2 ml, a b s o r b a n c e by t h e r e s u l t a n t b o r i c a c i d - a z o m e t h i n e complex was l i n e a r l y r e l a t e d t o a l i q u o t boron c o n c e n t r a t i o n r a n g i n g from 0.5 t o 8 ppm. The r e a c t i o n complex

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obeyeu t h e Lambert-Beer

l a w w i t h i n t h e r a n g e of b o r o n c o n c e n t r a t i o n and

aliquot size investigated. S i g n i f i c a n t e f f e c t s of t e m p e r a t u r e and time (FiF;.

1) were o b s e r v e d

when r e a c t i o n m i x t u r e s of w a t e r and 2 ppm boron s t a n d a r d were immediately

0.4
6C

0.3

*
(v

s
0.2

1 a

i
0.1

10

20
FIG. 1

30
Time (min)

b0

50

LfiiLt

of t e u p c r a t u r e a u . t i c i e on c o l o u r development (2 ppm boron)

BORON IN SOILS AND PLANTS

p l a c e d i n t o t h e r e f e r e n c e and sample c u v e t t e s , m a i n t a i n e d a t v a r i o u s

563

t e m p e r a t u r e s i n t h e s p e c t r o p h o t o m e t e r ' s c u v e t t e compartment,and r e l a t i v e a b s o r b a n c e was monitored a t v a r i o u s times d t i r i n g t h e f i r s t h o u r . Absorbance reached a s t a b l e maximum a f t e r 30 min a t 2 3 O C .

A t 6OC,

a b s o r b a n c e c o n t i n u e d t o i n c r e a s e a n d , a f t e r 1 h r , exceeded t h e nlaximum observed a t 2 3 O C . On t h e o t h e r hand, a s t a b l e e q u i l i b r i u m w a s e s t a b l i s h e d However, a b s o r b a n c e was o n l y h a l f t h a t o b t a i n e d

A s i m i l a r u n d e s i r a b l e l o s s of s e n s i t i v i t y was

w i t h i n 10 min a t 4 5 O C .

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a f t e r 30 ruin a t 2 3 O C . r e p o r t e d by Basson g

A.2when

t e m p e r a t u r e exceeded 4 O o C d u r i n g a n When a r e a g e n t b l a n k , p r e p a r e d w i t h

u n s p e c i f i e d c o l o u r development p e r i o d .

water, was p l a c e d i n t h e sample c u v e t t e and a b s o r b a n c e r e l a t i v e t o water o r a i r i n t h e r e f e r e n c e c u v e t t e was monitored w i t h o u t t e m p e r a t u r e c o n t r o l , a b s o r b a n c e a e c r e a s e d w i t h t i m e and a s i g n i f i c a n t d e c r e a s e was o b s e r v e d w i t h i n 5 min. However, a b s o r b a n c e remained c o n s t a n t when t e m p e r a t u r e was U n l e s s t e m p e r a t u r e was r e g u l a t e d , c o n t i n u e d e x p o s u r e

regulated at 23OC.

t o t h e s p e c t r o p h o t o n i e t e r ' s l i g h t beam i n c r e a s e d t e m p e r a t u r e , a n d measurement was a f f e c t e d . When c o l o u r development of boron s t a n d a r d s was e x t e n d e d t o

1, 2 ,

OK

4 h r , absorbance r e l a t i v e t o simultaneously prepared reagent

b l a n k s d i d n o t d i f f e r from c o r r e s p o n d i n g a b s o r b a n c e measured a t 30 min. However, r e l a t i v e t o f r e s h r e a g e n t b l a n k p r e p a r e d 30 min b e f o r e measurement, a b s o r b a n c e by b l a n k s and s t a n d a r d s d e v e l o p e d f o r 1 o r 2 h r

increased slightly.

O n t h e o t h e r hand, d e c r e a s e d a b s o r b a n c e r e l a t i v e

t o a f r e s h b l a n k was o b s e r v e d when b l a n k s anti s t a r . d a r d s were d e v e l o p e d f o r 4 h r and t h e d e c r e a s e was g r e a t e s t a t h i g h e r b o r o n c o n c e n t r a t i o n s . E x t e n d i n g t h e development p e r i o d beyond 30 min, such a s t h e 1 o r 2 hr p e r i o d s recomnended by w o l f 5 , p r o v i d e d no a d v a n t a g e . Optimum s e n s i t i v i t y

and c o n v e n i e n c e were o b t a i n e d when c o l o u r was d e v e l o p e d a t room

564

JOHN, CHUAH, AND NEUPELD

t e m p e r a t u r e (23OC), a b s o r b a n c e was measured a f t e r 30 min a t t h e same t e m p e r a t u r e and f r e s h r e a g e n t b l a n k s were s u b s t i t u t e d a t i n t e r v a l s . Absorbauce by complexes w i t h 2 ppm b o r o n s t a n d a r d i n c r e a s e d c o n c e n t r a t i o n of azomethine-H
(Fig. 2).

as

r e a g e n t was i n c r e m e n t e d t o 0.8 g / 100 m l

Absorbance remained r e l a t i v e l y unchanged when more c o n c e n t r a t e d However, u n a e s i r a b l c - t u r b i d i t y r e s u l t e d when i t s When a d o p t i n g t h i s method f o r l a r g e

r e a g e n t was used.

c o n c e n t r a t i o n exceeded 1.0 g / 100 m l .

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nunlbers of samples, s u c h as i n c o r p o r a t i n g boron d e t e r m i n a t i o n a s a r o u t i n e a n a l y s i s in soil and p l a n t material t e s t i n g programs, t h e economics of u s i n g r e l a t i v e l y e x p e n s i v e azomethine-H must be c o n s i d e r e d . r e a g e n t c o n c e n t r a t i o n of 0.8 g Although

/ 100 m l p r o v i d e d t h e b e s t s e n s i t i v i t y ,

0.4

0.3
0

i !

o.2

0.1

0.2

0.4

0.6

0.8

1.o

1.2

Azomethine H Concentration (dl00ml)

FIG. 2
E f f e c t of azomethino-H r e a g e n t c o n c e n t r a t i o n on c o l o u r (2ppm boaon)

BORON I N SOILS AND PLANTS

u s e of 0 . 4 5 g i.e.,

565

1 U 0 nl gave a d e q u a t e s e n s i t i v i t y f o r r o u t i n e a n a l y s i s ,

0 . 0 1 change i n a b s o r b a n c e r e p r e s e n t e d a 0 . 0 6 ppm Change of b o r o n

c o n c e n t r a t i o n i n sample a l i q u o t .

The c o n c e n t r a t i o n of 0 . 4 5 g

/ 100 m l

was selected f o r practical adaptability.

A s t u d y of t h e e f f e c t of v a r y i n g t h e c o n c e n t r a t i o n of L - a s c o r b i c

a c i d i n t h e a z o m e t h i n e r e a g e n t i n d i c a t e d t h e p r e s e n c e of 1, 2 . 5 , o r 5 % a s c o r b i c a c i d w a s b e n e f i c i a l but i t s absence
OK

c o n c e n t r a t i o n s of 7 . 5 and

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10% u i d n o t p r o v i u e a s t a b l e r e a g e n t .

S i n c e c o n c e n t r a t i o n s of 2.5 o r 5%

d i d n o t p r o v i d e a d d i t i o n a l s t a b i l i t y , u s e of 1% s c o r b i c a c i d w a s a d o p t e d . a Whereas c o n s i d e r a b l e loss of s e n s i t i v i t y was o b s e r v e d a f t e r azomethine-1 r e a g e n t was s t o r e d a t room t e m p e r a t u r e ( 2 3 O C ) f o r 5 d a y s , no r e d u c t i o n of s e n s i t i v i t y was found when i t had b e e n s t o r e d i n a r e f r i g e r a t o r a t 4OC f o r 15 d a y s . of a a s s o n Although t h e s e r e s u l t s c o n f i r m e d t h o s e

a b s o r b a n c e by r e a g e n t b l a n k s p r e p a r e d w i t h r e a g e n t t h a t

had been s t o r e d a t 4OC f o r one week d i f f e r e d s l i g h t l y from a b s o r b a n c e by

one p r e p a r e d w i t h f r e s h azomcthinc-H r e a g e n t .
azonietliinc-11

The same b a t c h of

r e a g e n t musl: b e used f o r b o t h t h e s a m p l e s and t h e c o r r e s p o n d i n p New r e a g e n t s h o u l d b e p r e p a r e d e a c h week and s t o r e d

calibration standards. uncier r e f r i g e r a t i o r , .

A s t u d y of the method's

t o l e r a n c e t o i n t c r f e r e n c e from s e l e c t e d i o n s

present

ii;

s o i l s , p l a n t n a t e r i a l s and common e x t r a c t s and d i g e s t s i n d i c a t e d

c a l c i u m , magnesium, p o t a s s i u m , sodiuin, n i t r a t e , c h l o r i d e , a c e t a t e , c i t r a t e o r o x a l a t e i o n s (to maximum 10,000 ppni c o n c e n t r a t i o c s i n v e s t i g a t e d ) i i a d e f f e c t on t h e u e t e r n i n a t i o u of a 2 ppn boroi; s t a n d a r d (Table 1 ) . C o n c e n t r a t i o n of p e r c h l o r a t e o r a r s e n a t e i o n s t o 1 0 , 0 0 0 p p n were a l s o p e r m i s s i b l e when l e s s t h a n 5% e r r o r was c o n s h e r e d t o l e r a b l e , b u t f l u o r i d e i o n c o i l c e n t r a t i o n c o u L n o t exceed 5 , O O C ppn. boron stai:darL Iflien 1-nl a l i o u o t s of 2 p p r ~ no

c o n t a i n c c : u1i t o 3 , 0 0 0 ppm alur.iinum, 200 ppm f e r r i c o r 2 , 5 0 0

1;il

ppn c u p r i c i o n , use o t 2

of t:ie b u f f e r maskin::

solution c o n t a i n i n g

566
TABLE 1

JOHN, CHUAR, AND NEUFELD

Tolerance L i m i t s f o r Selected Ions

Ion

Source

Concn, ppm i n 2 ppm boron

Error

T:
0

calcium magnesium

Ca (NO3 )

10,000
10,000 10,000 10,000 10,000

M i n d i l u t e {NO3 g KC 1
NaCl
IQ03

0
0
0

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potassium
sod ium

niLrata c ti l o r i d e acetate c i tra t e oxalate perctilora te arsenate f luoridr

dlUrlillULl

0
0

HC1 CH3COONM4
(NH4) 2HC6H507

10,ooc
10,000
10,000
10,000

0
0

(114) p 2 0 4 .H20 HC104 ha2HAs04. 7H20 NH4F

A l C l .6H20

0 3 3

10,000 10,000 5,000

-5
2
5 5

ferric rupric

3 FeMt4(S04)2.12H20

3,000

2CO
2,500

CuO i n u i l u t e HC1

U.077

fi

EbTA (disodium s a l t ) and 2 m l of azomethine-H

reagent containing Relative t o t o l e r a n c e may

1/. a s c o r b i c a c i u e f f e c t i v e l y s u p p r e s s e d i n t e r f e r e n c e .
t o l e r a b l e c o n c e n t r a t i o n s g i v e n by Basson

a,, improved

ue d u e t o tire g r e a t e r d i l u t i o n of t h e sample a l i q u o t and h i g h e r c o i i c e n t r a t i o n of ODTA (disodium s a l t ) .

No i n t e r f e r e n c e problems a r e

Lxpecteu when b o r o n is d e t e r m i n e d i n most s o i l and p l a n t e x t r a c t s s i n c e c o n c e n L r a t i o n s of t h e i o n s s t u d i e d a r e g e n e r a l l y below t h e d e l i n e a t e d tolerance levels. The a c c u r a c y of t h e proposed azomethine-11 method u n d e r p r a c t i c a l a p p l i c a t i o n s was i n d i c a t e u by b o r o n d e t e r m i n a t i o n s b e f o r e and a f t e r a u d i t i o n of known amounts t o a l f a l f a e x t r a c t . s o i l e x t r a c t and e f f l u e n t

BORON IN SOILS AND PLANTS

( T a b l e 2). When means of 3 r e p l i c a t e s were c o n s i d e r e d , t h e p e r c e n t a g e

567

error between d e t e r m i n e d boron c o n c e n t r a t i o n s and c a l c u l a t e d boron

c o n c e n t r a t i o n s was less t h a n 3%. When boron i n a l f a l f a , Monroe and Ladner s o i l s , sewage s l u d g e and e f f l u e n t w a s d e t e r m i n e d by t h e proposed azomethine-H method and t h e carmine methoda, r e s u l t s of t h e two methods were i n c l o s e a g r e e m e n t ( T a b l e 3 ) . S n a l l e r w i t h i n - s a m p l e s t a n d a r d d e v i a t i o n s (SD) c a l c u l a t e d from d u p l i c a t e

Downloaded by [Ohio State University Libraries] at 09:05 24 March 2012

b o r o n d e t e r m i n a t i o n s f o r e a c h of 4 r e p l i c a t e e x t r a c t s o r p o r t i o n s of t h e s a m p l e , and smaller o v e r a l l s t a n d a r d d e v i a t i o r i s were a s s o c i a t e d w i t h t h e proposed method. method method. These r e s u l t s i n d i c a t e d t h e p r e c i s i o n of t h e proposed

is c o n s i d e r a b l y s u p e r i o r t o t h a t o b t a i n e d u s i n g t h e carmine
Another a d v a n t a g e of t h e azomethine-H method
i 6

elimination

Of

concentrated s u l p h u r i c a c i d

reagent.

The d e s c r i b e d method p r o v i d e d r a p i d and r e l i a b l e b o r o n d e t e r m j n a t i o n s f o r s o i l and p l a n t t i s s u e t e s t i n g programs and s o i l f e r t i l i t y and p l a n t n u t r i t i o n research.

TABLE 2 Accuracy o f Boron Determined by t h e Proposed Azomethlne-H Method When Known Amounts Were Added t o S o l u t i o n

Sample

Extraction

w'v

ratio

ppni boron on sample b a s i s Before After Calculated

% Error

Alfalfa tops Monroe soil Effluent

N - HCl

dry ash,

1:5

37.5

42.6

42.5

0.2

hot water

1:2

1.04

2.04

2.04

0.0

-----

---

0.7b

1.82

1.78

2.2

568
TABLE 3

JOHN, CWAH. AND NEUFELD

Comparison of t h e Proposed Azomethine-H Method and t h e Carmine Method

Sample

Extraction

w'v

ratio

Azome thine-A Mean SD

Carmine Mean SD

Alfalfa tops Monroe

dry ash, - 11c1 N hot

1:5
1:2

37.4

ppm boron o n sample b a s i s 0.181 37.3 1.634

1.04

0.063

0.97

0.062

soil

water
110 t

Downloaded by [Ohio State University Libraries] at 09:05 24 March 2012

Ladner

soil
Sewage sludge Effluent

water
hot water

1:2

2.10

0.041

2.34

0.126

1:2

1.22

0.068 0.016
0.091

1.34 0.70

0.081

-----

---

0.78

0.031

Overall

0.734

REFEr3lNCES

1.
2.

Soil and Fedd T e s t i n g L a b o r a t o r y , F i e l d Crops Branch, B r i t i s h Columbia

Department of A g r i c u l t u r e , Kelowna, B r i t i s h Columbia, Canada. W.D. Basson, K.G. Bohmer and D . A . Stanton, Analyst,

94, 1135

(1969).

3. 4.

V. Petrovsky, T a l a n t a ,

lo, 175

(1963).

l.M. S h a n i n a , N.L. Gel'man and V . S . M i k h a i l o v s k a y a , J. A n a l y t . Chem. USSR, t r a n s l a t e d e d i t i o n , 22, 663 (1967).

6 . I l o l f , Comm. Soil S c i . P l a n t A n a l . ,

5.

2, 363

(1971).

6.
7.
8.

E1.h. J O ~ I I , Soil S c i . SOC. Am. P r o c . , 37, 332 (1973).

Azomethine-11 r e a g e n t o b t a i n e d from P i e r c e Chemical Co., I l l i n o i s 61105. Fackford,

J.T. H a t c h e r and L.V.

Wilcox, Anal. Chem., 22, 567 (1950).

R e c e i v e d March 4, 1975 A c c e p t e d A p r i l 4, 1975