agilent 6820 · 2017. 5. 31. · james d. mccurry, “running astm methods d 4815 and d5580 on a...
TRANSCRIPT
Agilent 6820�� !"#$%�� !"#
��
��
�� !"�� !�� !
�� !"#$%&'() 412 � 200131
��
�� !"#$%&�� !
�� !"#$%&' 118�� ! 16 � 100022
��
�� !"#$%& Agilent 6820�� !"#$�� !"
�� !"#!$%&'�� !"#!$ (MTBE)��� !
�� (ETBE)��� ! " (TAME)��� ! (DIPE)���
�� �� !�� !�� !�� !�� !"# $�
�� !"�� !"#$#%& (DME)�
��
�� !"#$%&'(")*+,-.!,/01
�� !�� !"#$%&�� !"#$%&'(
�� !"#$%&'()*+,-./01234
�� !�� !�� !�� !"#$%&'��
�� !"#$%&'() *+,%-./��
�� !"#$%&'()*+,-.�� !"#
��� !GB17930-1999�� !"#1�� ��
�� !"#$%&2.7% (m/m)��� !2003�1
�1�� !"#$%&'(�� !"#$%&'(
�� !"#$%&&'()*+,-./() SH/
T0663-1998 2��� !"#$%ASTM D4815 3��
�� ASTM D4815�� !"#$%&'%()*
��
�� !
�� !"#$%&'��/�� !"#$%&'(
�� ! (FID) � Agilent 6820�� !"#$%&
�� !"�#$% 1,2,3- � (2-�� !�) ��
(TCEP) �� !"#$�� !HP-1�� !"#
�� �� !"# 1 �� �� !"#$%&'
�� !"�� !"#$%&'()* (G4323A)�
�� !�
G1180A 6820�� !"# 1
161 �� /�� !"#$%& 1
215 �� !"#$%& 2
302 �� !"#$% 1
751 �� !"# 1
800 �� 1
872 �� 530�� !"# 2
870 �� ! 1
874 �� !"#$%&% 1
335 Cerity NDS ��(��) 1
G4323A �� !"#$%& 1
��
19095Z-123 �� !HP-1 30 m, 0.53 mm, 2.65 m 1�� !"56 cm x 1/16" TCEP(20%) 1
�� !
���� !"
�� !
1��� !"�� ! "#$�� !"#$%�
�� !" TCEP�� !�� !"#$%&
TCEP�� !"#$�� !"#$%&'()
�� !"#$%&�� !"�OFF�����
� 1A��
� 1. �� !
2��� !"#$%&�� !" (DIPE) �� !
��� (MTBE) �� !"#$%�� !�ON�
�� (�� 1B) �� !"#$%&'()*+
�� !HP-1�
3��� !"!# (TAME) �� !"#$%��
�� !"#$%��OFF���� !"#$
� 1. A � OFF � 1. B� ON � 1. C � OFF
TCEP
HP-1
FID
OFF
HP-1
TCEP
FID
TCEP
HP-1
OFFFID
12
3
4
56
7
8
910
12
3
45
67
8
9
10
ON
12
3
4
56
7
8
910
2
�� !"#
�� !"#$%&'()�� !"#$%C5��
�� !"#$%&'()*�� C4�� !"#
�� !"#$%&�� !"�� !"#$%��
�� !"#$%
�� MTBE�DIPE�DME�� !"# (MCP) ��
�� !"#$%&'()*+,&'-�� !"
��0.18�0.34�� �� !"#$%&'(2��
0.22�� �� !"�� !"#�� TCEP��
���� !"#$%&�� MTBET �DIPE��
�DIPE�� !"#�� !"#$%&'0.28��
�� !"# Cerity NDS�� !"#
�� ! 0.22�� �� MTBE�DIPE�� !�0.22�� ���� !"#$%&'��� TCEP�� !"� MTBE�DIPE ��� TCEP��
�� Agilent 6820
�� !"#$%& Cerity NDS
�� �� /�� !"#200���� !15:1
�� FID�250���� N2�18 mL/min
�� 60��(6 min)�2�/min�75��5�/min�115�
�� 60�
�� !" N2, 3 mL/min
�� !"# N2, 3.5 mL/min
�� ! 350 mL/min
�� ! 40 mL/min
�� ! 0.21 min 1
�� ! TCEP�� !"� 560 mm��� 1.6 mm��� 0.38 mm
�� HP-1�30 m�0.53 mm�2.65 m
� 1��� !"#$%&'()*+
� 2. �� !"#
� DIPE�� !"�� !"#$% 0.28�� �0.28�� MTBE�� !TCEP����� ! DIPE �� TCEP ��
�� !
�� !"# 2��
�� ! ��
��
(Are
a)
Area, MTBE/DME
Area, DME/DME
Area, DIPE/DME
Area, MCP/DEM
3.5
3
2.5
2
1.5
1
0.5
0
0.18 0.2 0.22 0.24 0.28 0.3 0.32 0.34
3
��
�� !"#$%&'()*�� !"#$%&'
�� !"#$0.1�0.5�2�5�10�15�20% (m/m)
�� !"#$%�� !"#$�� !�� !"
�� ! /�� !"#��Y���� �� !"
�� !/�� !"#��X�� !"#$%&'
�� !"#
�� !"
�� !
�� !"#$%&'()*+�,-%)./��
�� !"#0.999�� !"#$�2�� !"#
�� !�� !"#$%&'()
�� !"#$%&'�� !Y�� bi�� !"
�� !"#$�� !"#$�wi��0.1% (m/m)
��Ai�� ! 0�Y�� !"#$%�&'()
wi = (bi/mi)�(ws/wg)� 100-----------(1)
�� wi�� !"# i�� !"#$ASTM4815�
�� !wi�� 0.1% (m/m)�
ws�� !"#$%&'()g�
wg�� !"#$g�
��2�� !"#bi=0.0028�mi=1.9754��� !
�� !"#$%&' 0.5 mL �� (ws=0.4 g) � 9.5
mL �� (wg=7 g)��� !"#$ (1) �� !
wi=(0.0028/1.9754)�(0.4g/7g)� 100=0.008% (m/m)
wi=0.008% (m/m) ��� 0.1% (m/m)��� !"
����bi�� !"#$%&�� !"#$%&'
�� !"#$%wi�� 0.1% (m/m)�
� 2. �� !"#$%
�� !�� / �� (�� �!")
�� !"#��
/�
�
3.5
3
2.5
2
1.5
1
0.5
00 0.5 1 1.5 2
y = 1.975x + 0.0028R2 = 1
4
�� !"#$%&'
�3�� !"�� !" #$%&'(13�� �
�� !"#$%&�'(
� 4�� !"#$%&�� !"#$%&'()
���� !"#$ASTMD4815 (� SH/T0663) �
��
1. ��
2. ��
3. �� 4. �� 5. �� 6. �� ! ��
7. �� 8. �� ! 9. �� 10. �� 11. �� � �� 12. �� 13. �� !"14. ��
� 3. ���� !"#$%!&'()
n
4500
4000
3500
3000
2500
2000
1500
1000
500
0
�� �� ! (5�� ) ASTMD4815 (� SH/T0663) �� !"
�� !% (m/m) �� ��
�� 7.974 0.225 0.09(X0.59) = 0.306
�� 0.539 0.026 0.06(X0.61) = 0.041
�� 7.958 0.012 0.04(X0.56) = 0.128
�� 0.491 0.023 0.04(X0.56) = 0.027
�� 5.008 0.033 0.03(X0.57) = 0.075
�� 2.008 0.004 0.03(X0.61) = 0.046
�� 1.996 0.008 0.08(X0.56) = 0.119
�� 1.851 0.015 0.04(X0.61) = 0.058
�� 0.488 0.004 0.06(X0.61) = 0.039
�� !�" 0.499 0.031 0.05(X0.56) = 0.034
�� !" 1.867 0.021 0.08(X0.56) = 0.114
�� ! " 16.668 0.278 0.05(X0.70) = 0.358
��X�� !"#!$%&'()
�� !�� !"#$��%&'()�*+,-./-0123 !4567*89:;<=>4?@AB1CDEFGHI:�J�SH/T0663��� !"#$%&'()*+�� !"#)
5
0 2 4 6 8 10 12 14 16 min
� 4. �� !"
Cerity NDS
Cerity NDS�� !"#$%&'()*+�� !
�� !��"#$%&'()*+,-./��
�� !"#$ Cerity NDS�� !"#$%
1
2
3
4
5
6
78
910
11
12
13
14
www.agilent.com/chem
�� !"#$%&'()*+,-.�� !"�� !"#$%&'()*+,-./
��
�� !"#$�� !"#$%&'�� !"#$
©�� !"#$%&'()2004 �
�� !
2004 � 6 � 1 �
5989-1337CHCN
��
�� Agilent 6820�� !" (GC) �� !"#$
�� !"�� !"#$%�� !ASTM D4815
�� !"#$%&'%(�� !"#$%&��
�� !"#$%&'Cerity NDS�� !"#$%�
�� !"#$�� !"�� !"#$%&'()
�� 0.999�� �� !"#$%&'()*+"
���� !"#$%ASTM D4815���� !"
�� !"#$%&'() SH/T0663��� !
�� !
1. �� !"#$$%&'GB17930-1999�� !
��
2. �� !"#$%&'()*+,SH/T0663-1998
�� !"#$%&$'()(�� !")
3. ASTM D4815 Standard Test Method for
Determination of MTBE, TAME, DIPE, tertiary-
Amyl Alcohol and C1-C4 Alcohols in Gasoline by
Gas Chromoatography
4. James D. McCurry, “Running ASTM Methods D
4815 and D5580 on a Single Agilent 6890N Gas
Chromatograph With Nitrogen Carrier Gas”,
Printed in the USA March 17, 2003 5988-9153EN